CN114634372A - Porous ceramic material for atomizing core, porous ceramic body, ceramic atomizing core, preparation method and electronic cigarette - Google Patents
Porous ceramic material for atomizing core, porous ceramic body, ceramic atomizing core, preparation method and electronic cigarette Download PDFInfo
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- CN114634372A CN114634372A CN202210306536.0A CN202210306536A CN114634372A CN 114634372 A CN114634372 A CN 114634372A CN 202210306536 A CN202210306536 A CN 202210306536A CN 114634372 A CN114634372 A CN 114634372A
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000003571 electronic cigarette Substances 0.000 title claims abstract description 14
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- 239000000843 powder Substances 0.000 claims abstract description 77
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- 229910052906 cristobalite Inorganic materials 0.000 claims description 14
- 238000002844 melting Methods 0.000 claims description 14
- 239000000377 silicon dioxide Substances 0.000 claims description 14
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- 229910002804 graphite Inorganic materials 0.000 claims description 6
- 239000010439 graphite Substances 0.000 claims description 6
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- 238000002791 soaking Methods 0.000 claims description 5
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- -1 polypropylene Polymers 0.000 claims description 4
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- 238000004321 preservation Methods 0.000 claims description 4
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 claims description 4
- 229910000391 tricalcium phosphate Inorganic materials 0.000 claims description 4
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 4
- 239000003502 gasoline Substances 0.000 claims description 3
- 239000003350 kerosene Substances 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 3
- 229910052878 cordierite Inorganic materials 0.000 claims description 2
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 claims description 2
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 claims description 2
- 238000003801 milling Methods 0.000 claims description 2
- 229910052863 mullite Inorganic materials 0.000 claims description 2
- 229910000623 nickel–chromium alloy Inorganic materials 0.000 claims description 2
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims 1
- 239000011148 porous material Substances 0.000 abstract description 13
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- 235000002637 Nicotiana tabacum Nutrition 0.000 description 20
- 230000000052 comparative effect Effects 0.000 description 11
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- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 8
- 239000000203 mixture Substances 0.000 description 7
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- 229910001120 nichrome Inorganic materials 0.000 description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 2
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- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
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- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
- C04B38/063—Preparing or treating the raw materials individually or as batches
- C04B38/0635—Compounding ingredients
- C04B38/0645—Burnable, meltable, sublimable materials
- C04B38/068—Carbonaceous materials, e.g. coal, carbon, graphite, hydrocarbons
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24F—SMOKERS' REQUISITES; MATCH BOXES; SIMULATED SMOKING DEVICES
- A24F40/00—Electrically operated smoking devices; Component parts thereof; Manufacture thereof; Maintenance or testing thereof; Charging means specially adapted therefor
- A24F40/40—Constructional details, e.g. connection of cartridges and battery parts
- A24F40/46—Shape or structure of electric heating means
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24F—SMOKERS' REQUISITES; MATCH BOXES; SIMULATED SMOKING DEVICES
- A24F40/00—Electrically operated smoking devices; Component parts thereof; Manufacture thereof; Maintenance or testing thereof; Charging means specially adapted therefor
- A24F40/70—Manufacture
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- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
- C03C3/097—Glass compositions containing silica with 40% to 90% silica, by weight containing phosphorus, niobium or tantalum
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Abstract
The invention provides a porous ceramic material for an atomizing core, a porous ceramic body, a ceramic atomizing core, a preparation method and an electronic cigarette, and relates to the technical field of electronic cigarettes. Porous ceramic material for atomizing core, comprising aggregateRaw materials such as pore-forming agent and organic binder, wherein the aggregate comprises glass powder with specific softening point and SiO-containing2Ceramic powder, the glass powder and SiO-containing2The ceramic powder has good compatibility with SiO-containing2The ceramic powder is mixed with the pore-forming agent and the organic binder in a certain proportion to serve as ceramic aggregate, so that the porous ceramic body prepared from the porous ceramic material for the atomizing core has the advantages of small shrinkage rate, high porosity, high strength and smooth inner wall of pores, and the oil absorption and oil conduction speed is high. The invention provides a porous ceramic body which is prepared from the porous ceramic material. The invention provides a ceramic atomizing core which is prepared from the porous ceramic body.
Description
Technical Field
The invention relates to the technical field of electronic cigarettes, in particular to a porous ceramic material for an atomizing core, a porous ceramic body, a ceramic atomizing core, a preparation method and an electronic cigarette.
Background
The porous ceramic atomizing core is a key core component of the electronic cigarette. From the structure of the atomizing core appearance, it can be divided into two parts: porous ceramic body and metal heating electrode. The metal heating electrode mainly has the function of enabling the electrode with a certain resistance value to perform self-heating under the action of an external power supply, providing a uniform and stable heat source and atomizing the tobacco tar near a contact interface of the electrode and the ceramic. The role of the porous ceramic body in the electronic cigarette mainly comprises:
(1) oil storage: store a certain amount of tobacco tar inside the ceramic body, when the surface circuit heating atomizing, the tobacco tar of the inside ceramic body moves towards the heating surface rapidly, makes smog produce.
(2) Oil absorption and oil guiding: when the tobacco tar on the heating surface is consumed, the tobacco tar in the ceramic body can be quickly supplemented to the heating surface, and meanwhile, the tobacco tar can be quickly supplemented to the inside of the ceramic body by the contact part of the other surface of the porous ceramic and the tobacco tar; when the tobacco tar is not consumed in time, local scorching can occur. Under a certain tobacco tar formula system, the oil absorption and oil guide speed is mainly related to factors such as the porosity size of the porous ceramic, the pore structure, the pore wall state, the matching property of the ceramic material and the tobacco tar, and the like.
(3) Dividing the size of tobacco tar liquid particles: after the tobacco tar passes through the pore canal of the porous ceramic, the tobacco tar can be cut into a plurality of small liquid drops by the porous ceramic, and only the small liquid drops can reach the atomizing surface, so that the tobacco tar can quickly generate smoke at the temperature of the atomizing surface.
The size of the smoke amount is an important index for evaluating the electronic cigarette. The amount of the smoke is generally related to the atomizing core, the tobacco tar formula (the proportion of the propylene glycol and the glycerin), and the actual heating power in the smoking process. Wherein, atomizing core is the key: under the condition of large smoke quantity, the vaporization speed of the tobacco tar is accelerated, and if the tobacco tar at the interface cannot be supplemented in time, local overhigh temperature can be caused, so that the core is burnt. How to reduce the burnt core under the large smoke quantity is a problem which needs to be solved urgently in the industry.
At present, the preparation method of the porous ceramic body mainly adopts ceramic powder such as diatomite, quartz sand, alumina, silicon carbide and the like as ceramic aggregate, sodium silicate as a binder, organic matters such as starch, wood dust and the like as pore-forming agents, and the porous ceramic body is formed by molding modes such as dry pressing, hot pouring, injection and the like, and is prepared by procedures such as degreasing, sintering and the like.
When the porosity of the traditional porous ceramic material for the atomizing core is more than 60 percent, the strength of the ceramic body is reduced, and the phenomena of powder falling and even fragmentation are easy to occur in the production and use processes of the atomizing core. Under the influence of the characteristics of the ceramic material, the microscopic state of the pore canal and other factors, the oil absorption and oil guide speed of the ceramic is slow, the phenomenon of 'core pasting' is easy to occur due to insufficient oil supply, and the atomization amount is greatly attenuated in a long-opening (more than 300 openings) state, so that the taste experience of a user is influenced.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The first purpose of the invention is to provide a porous ceramic material for an atomizing core.
The second object of the present invention is to provide a porous ceramic body obtained by using the above porous ceramic material for an atomizing core.
The third object of the present invention is to provide a method for producing the above porous ceramic body.
A fourth object of the present invention is to provide a ceramic atomizing core.
The fifth purpose of the invention is to provide a preparation method of the ceramic atomizing core.
A sixth object of the present invention is to provide an electronic cigarette.
In order to achieve the purpose, the technical scheme of the invention is as follows:
the invention provides a porous ceramic material for an atomizing core, which comprises the following components in percentage by mass based on 100% of the mass fraction of the porous ceramic material:
40-55% of aggregate, 35-45% of pore-forming agent and 10-20% of organic binder;
wherein the aggregate comprises glass powder and SiO2Ceramic powder of said SiO-containing2The mass ratio of the ceramic powder to the glass powder is 1: (0.5-1), and the softening point of the glass powder is 950-.
Further, on the basis of the above technical scheme of the present invention, the glass frit comprises the following raw materials by mass percent, calculated as 100% by mass of the glass frit:
SiO2 60-80％，Al2O3 2-10％，Na2CO3 0-5％，Ca3(PO4)2 1-10％，MgO 1-5％，H3BO35-15％，TiO20-2% and ZnO 0-5%.
Further, on the basis of the above technical scheme of the present invention, the preparation method of the glass frit comprises the following steps:
(a) mixing and grinding raw materials of glass powder, then carrying out high-temperature melting, and quenching the obtained glass liquid to obtain glass slag;
(b) grinding the glass slag to obtain glass powder;
preferably, in step (a), grinding to a particle size D50 ≤ 10 μm;
preferably, in the step (a), the melting temperature is 1500-;
preferably, in step (a), the quenching is water quenching;
preferably, in step (b), the milling is carried out to a particle size D50 of 10 to 30 μm.
Further, on the basis of the technical scheme of the invention, the SiO-containing material2The ceramic powder comprises any one or combination of at least two of diatomite, quartz sand, mullite or cordierite, preferably diatomite;
preferably, the pore-forming agent is graphite, and the granularity D50 of the graphite is 10-30 μm;
preferably, the organic binder comprises the following raw materials in percentage by mass, calculated by taking the organic binder as 100% in percentage by mass:
55-75% of semi-refined paraffin, 5-20% of carnauba wax and 10-30% of polypropylene.
The invention provides a porous ceramic body which is made of the porous ceramic material for the atomizing core;
the porous ceramic body has an oil absorption rate of 10-14 mg/s.
Further, on the basis of the technical scheme of the invention, the compressive strength of the porous ceramic body is 17-26 MPa;
and/or the porous ceramic body has a porosity of 62-75%.
The invention provides a preparation method of the porous ceramic body, which comprises the following steps:
mixing the raw materials of the porous ceramic material for the atomizing core, and performing injection molding to obtain a green body;
degreasing the green body, and sintering to obtain a porous ceramic body;
preferably, the mixing temperature is 120-160 ℃, and the mixing time is 2-5 h;
preferably, the injection temperature is 140-;
preferably, the degreasing treatment comprises the step of soaking and degreasing the green body in a degreasing solvent;
preferably, the degreasing solvent comprises any one of paraffin oil, kerosene or gasoline;
preferably, the time of the degreasing treatment is 10-24 h;
preferably, the degreasing treatment is followed by a drying step before sintering;
preferably, the sintering temperature is 850-1050 ℃, the sintering time is 10-30min, the sintering atmosphere is vacuum, and the vacuum degree is less than or equal to 10 Pa.
The invention provides a ceramic atomizing core, which comprises the porous ceramic body and an electrode;
preferably, the electrode is a metal electrode.
The invention provides a preparation method of the ceramic atomizing core, which comprises the following steps:
printing the slurry for forming the electrode on the surface of the porous ceramic body, and then calcining to obtain a ceramic atomizing core;
preferably, the slurry is a metal slurry, preferably a nichrome slurry;
preferably, the calcination temperature is 850-1050 ℃, the heat preservation time is 10-30min, the calcination atmosphere is vacuum, and the vacuum degree is less than or equal to 10 Pa.
The invention provides an electronic cigarette, which comprises the porous ceramic body or the ceramic atomizing core.
Compared with the prior art, the invention has the following technical effects:
(1) the invention provides a porous ceramic material for an atomizing core, which comprises raw materials such as aggregate, pore-forming agent, organic binder and the like, wherein the aggregate comprises glass powder with a specific softening point and SiO-containing SiO2Ceramic powder, the glass powder and SiO-containing2Ceramic materialPowders (e.g. diatomaceous earth) having good compatibility with SiO-containing materials2The ceramic powder is mixed with the pore-forming agent and the organic binder in a certain proportion to serve as ceramic aggregate, so that the porous ceramic body prepared from the porous ceramic material for the atomizing core has the advantages of small shrinkage rate, high porosity, high strength and smooth inner wall of pores, and the oil absorption and oil conduction speed is high.
(2) The invention provides a porous ceramic body which is prepared from the porous ceramic material. In view of the advantages of the porous ceramic material, the porous ceramic body prepared by the porous ceramic material has small shrinkage, high porosity, high strength and smooth inner wall of pores, thereby having high oil absorption and oil guide speed.
(3) The invention provides a preparation method of the porous ceramic body, which has simple process and convenient operation and is suitable for industrial scale production.
(4) The invention provides a ceramic atomizing core, which comprises the porous ceramic body and an electrode. In view of the advantages of the porous ceramic body, the ceramic atomizing core prepared by the ceramic atomizing core can continuously suck 500 mouths under a certain (7.5W) power, the fluctuation of the average atomizing amount (TPM) is less than or equal to +/-10%, the mouthfeel is not obviously blurred, and the user experience is good.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the embodiments or the prior art descriptions will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a sectional view of a porous ceramic body produced by using a porous ceramic material for an atomizing core in example 16 of the present invention;
FIG. 2 is a perspective view of a ceramic atomizing core in accordance with one embodiment of the present invention;
FIG. 3 is a front view of the ceramic atomizing core of FIG. 2;
FIG. 4 is a side view of the ceramic atomizing core of FIG. 2;
FIG. 5 is a rear view of the ceramic atomizing core of FIG. 2;
FIG. 6 is a graph showing the change in the average amount of smoke in the ceramic atomizing core made of the porous ceramic material for the atomizing core in example 17 of the present invention.
Icon: 1-a porous ceramic body; 2-electrode.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to embodiments and examples, but those skilled in the art will understand that the following embodiments and examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. Those who do not specify the conditions are performed according to the conventional conditions or the conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
According to a first aspect of the invention, a porous ceramic material for an atomizing core is provided, which comprises the following components in mass fraction based on 100% of the mass fraction of the porous ceramic material:
40-55% of aggregate, 35-45% of pore-forming agent and 10-20% of organic binder;
wherein the aggregate comprises glass powder and SiO2Ceramic powder of SiO2The mass ratio of the ceramic powder to the glass powder is 1: (0.5-1), the softening point of the glass powder is 950-.
Unlike the traditional method of using diatomite, quartz sand, alumina, silicon carbide and other ceramic powder as ceramic aggregate, the porous ceramic material for the atomizing core in the invention mainly comprises SiO-containing aggregate2Ceramic powders (e.g., diatomaceous earth) and glass powders. It should be noted that, unlike the conventional commercially available glass powder (softening point of 500-. The softening point of the glass frit of the present invention needs to be limited within a certain range of values (950 ℃ C. and 1150 ℃ C.). Typical but not limiting softening points are 950 ℃, 960 ℃, 980 ℃, 1000 ℃, 1020 ℃, 1040 ℃, 1050 ℃,1060 deg.C, 1080 deg.C, 1100 deg.C, 1120 deg.C, 1140 deg.C or 1150 deg.C. If the softening point is less than 950 ℃ (e.g., < 900 ℃), the porous ceramic material is prone to premature glass melting during sintering at high temperatures, resulting in pore collapse and reduced porosity. If the softening point is too high (higher than 1150 ℃), the melting temperature is high, the production conditions are harsh, and the production is difficult; meanwhile, the softening point is too high, so that the ceramic has high burning temperature and high energy consumption in mass production.
Meanwhile, the aggregate contains SiO2The ratio between the ceramic powder and the glass powder needs to be limited within a certain range of values. Containing SiO2The typical but non-limiting mass ratio of ceramic powder to glass powder is 1: 0.5, 1: 0.55, 1: 0.6, 1: 0.65, 1: 0.7, 1: 0.75, 1: 0.8, 1: 0.85, 1: 0.9, 1: 0.95 or 1: 1. if the addition amount of the glass powder in the aggregate is too large (such as more than 50 percent), the pore canal of the prepared porous ceramic body is easy to collapse, and the window of the highest sintering temperature is narrow; if the amount of the glass frit added is too small, the resulting porous ceramic body may have poor roughness of the inner walls of the channels, insufficient strength, etc.
Glass powder and SiO-containing glass powder in the invention2Ceramic powders (e.g. diatomaceous earth) having good compatibility with SiO-containing materials2The ceramic powder is mixed in a certain proportion as ceramic aggregate, and in the process of sintering at high temperature, the glass powder is softened and wetted and is bonded with the diatomite, so that the prepared porous ceramic body has the advantages of small shrinkage, high porosity, high strength and smooth inner wall of pores, and the oil absorption and oil conduction speed is high.
The mass fractions of the aggregate, the pore-forming agent and the organic binder in the porous ceramic material for the atomizing core are also limited to a certain extent. The aggregate is typically, but not limited to, 40%, 42%, 44%, 45%, 46%, 48%, 50%, 52%, 54% or 55% by mass. Pore formers typically, but not by way of limitation, are 35%, 36%, 38%, 40%, 42%, 44%, or 45% by mass. The organic binder is typically, but not limited to, 10%, 12%, 14%, 15%, 16%, 18%, or 20% by mass.
The porous ceramic material for the atomizing core comprises raw materials such as aggregate, pore-forming agent, organic binder and the like, whereinThe aggregate comprises glass powder with specific softening point and SiO2Ceramic powder, the glass powder and SiO-containing2Ceramic powders (e.g. diatomaceous earth) having good compatibility with SiO-containing materials2The ceramic powder is mixed with the pore-forming agent and the organic binder in a certain proportion to serve as ceramic aggregate, so that the porous ceramic body prepared from the porous ceramic material for the atomizing core has the advantages of small shrinkage rate, high porosity, high strength and smooth inner wall of pores, and the oil absorption and oil conduction speed is high.
It is also to be noted that "comprising", "mainly made of … …" in the present invention means that it may comprise, in addition to the raw materials, other raw materials which impart different characteristics to the porous ceramic material for an atomizing core. In addition, the terms "comprising," "made primarily of … …," and "made of … …," as used herein, are intended to be interchangeable.
As an optional embodiment of the invention, the glass powder comprises the following raw materials in percentage by mass, calculated by taking the percentage by mass of the glass powder as 100 percent:
SiO2 60-80％，Al2O3 2-10％，Na2CO3 0-5％，Ca3(PO4)2 1-10％，MgO 1-5％，H3BO35-15％，TiO20-2% and ZnO 0-5%.
The glass powder of the invention is mainly made of SiO2、Al2O3、Ca3(PO4)2、H3BO3MgO and the like are taken as raw materials, and the prepared glass powder has the characteristics of high softening point and high strength through the cooperation of the raw materials.
Wherein, SiO2Typical but not limiting mass fractions are 60%, 62%, 65%, 66%, 68%, 70%, 72%, 75%, 76%, 78% or 80%; al (aluminum)2O3Typical but not limiting mass fractions are 2%, 4%, 5%, 6%, 7%, 8% or 10%; na (Na)2CO3Typical but not limiting mass fractions are 0%, 1%, 2%, 3%, 4% or 5%; ca3(PO4)2Typical but not limiting mass fractions are 1%, 2%, 4%, 5%, 6%, 7%, 8% or 10%; MgO typically but not limitatively in a mass fraction of 1%, 2%, 3%, 4% or 5%; h3BO3Typical but not limiting mass fractions are 5%, 6%, 7%, 8%, 10%, 11%, 12%, 14% or 15%; TiO 22Typical but not limiting mass fractions are 0%, 0.5%, 0.8%, 1%, 1.5%, 1.8% or 2%; typical but not limiting mass fractions of ZnO are 0%, 1%, 2%, 3%, 4% or 5%.
As an optional embodiment of the present invention, the method for preparing the glass frit comprises the following steps:
(a) mixing and grinding raw materials of glass powder, then carrying out high-temperature melting, and quenching the obtained glass liquid to obtain glass slag;
(b) and grinding the glass slag to obtain glass powder.
The glass powder with a specific softening point temperature is obtained by mixing and melting the raw materials of the glass powder at a high temperature to enable the raw materials to form glass-state substances, quenching and grinding the glass-state substances. The preparation method has simple process and convenient operation, and can be used for industrial mass production.
As an alternative embodiment of the invention, in step (a), grinding is carried out to a particle size D50. ltoreq.10 μm.
The raw materials are ground, so that the particle size of the raw materials is reduced, the mixing uniformity is improved, and the melting temperature in the process of preparing the glass powder can be reduced to a great extent.
As an alternative embodiment of the invention, in the step (a), the melting temperature is 1500-.
Typical but non-limiting melting temperatures are 1500 ℃, 1520 ℃, 1540 ℃, 1550 ℃, 1560 ℃, 1580 ℃, 1600 ℃, 1620 ℃, 1640 ℃ or 1650 ℃; typical but non-limiting incubation times are 2h, 3h, 4h, 5h or 6 h.
The specific manner of quenching is not limited, and as an alternative embodiment of the present invention, in the step (a), the quenching is water quenching.
As an alternative embodiment of the present invention, in step (b), grinding is carried out until the particle size D50 is 10 to 30 μm.
As a preferred embodiment of the present invention, the method for preparing the glass frit comprises the steps of:
(a) mixing the raw materials of the glass powder, adding pure water according to the proportion of 1 (1-1.5), placing the mixture into a ball mill for dispersing and crushing, controlling the ball milling speed and time, stopping grinding when the granularity D50 is less than or equal to 10 mu m, and drying;
filling the mixture into SiO2Melting the crucible at high temperature of 1500-1650 ℃, and carrying out heat preservation for 2-6h, and quenching the molten glass to obtain glass slag;
(b) and grinding the glass slag by a ball mill, wherein the material-water ratio is 1: 1-1.5, the ball milling time is 5-15h, the powder particle size D50 is controlled to be 10-30 mu m, and drying to obtain the glass powder.
In an alternative embodiment of the present invention, the pore-forming agent is graphite, and the particle size D50 of the graphite is 10 to 30 μm.
As an alternative embodiment of the invention, the organic binder comprises the following raw materials in percentage by mass, calculated by taking the organic binder as 100% in percentage by mass:
55-75% of semi-refined paraffin, 5-20% of carnauba wax and 10-30% of polypropylene.
A typical but non-limiting mass fraction of semi-refined paraffin is 55%, 56%, 58%, 60%, 62%, 65%, 66%, 68%, 70%, 72%, or 75%; a typical but non-limiting mass fraction of carnauba wax is 5%, 6%, 8%, 10%, 12%, 15%, 16%, 18%, or 20%; typical but not limiting mass fractions of polypropylene are 10%, 12%, 15%, 16%, 18%, 20%, 22%, 25%, 26%, 28% or 30%.
As an alternative embodiment of the present invention, the semi-refined paraffin wax is 56# semi-refined paraffin wax.
According to a second aspect of the present invention, there is provided a porous ceramic body made of the above porous ceramic material;
the porous ceramic body has an oil absorption rate of 10-14mg/s, typically but not limited to 10mg/s, 10.5mg/s, 11mg/s, 11.5mg/s, 12mg/s, 12.5mg/s, 13mg/s, 13.5 mg/s, or 14 mg/s.
The oil absorption rate of the porous ceramic body prepared by the conventional ceramic material is only 4-8mg/s generally, while the oil absorption rate of the porous ceramic body prepared by the porous ceramic material can reach 10-14 mg/s.
In view of the advantages of the porous ceramic material, the prepared porous ceramic body has small shrinkage, high porosity, high strength and smooth inner wall of pores, thereby having high oil absorption and oil guiding speed.
As an alternative embodiment of the present invention, the compressive strength of the porous ceramic body is 17 to 26 MPa;
and/or the porous ceramic body has a porosity of 62-75%.
The porous ceramic body typically, but not by way of limitation, has a compressive strength of 17MPa, 18MPa, 19MPa, 20MPa, 22MPa, 24MPa, 25MPa or 26 MPa. The porosity of the porous ceramic body is typically, but not limited to, 62%, 64%, 65%, 66%, 68%, 70%, 72%, 74%, or 75%.
According to a third aspect of the present invention, there is also provided a method for producing the above porous ceramic body, comprising the steps of:
mixing the raw materials of the porous ceramic material, and performing injection molding to obtain a green body;
and degreasing the green body, and sintering to obtain the porous ceramic body.
The preparation method has simple process and convenient operation, and is suitable for industrial mass production.
As an alternative embodiment of the invention, the mixing temperature is 120-160 ℃, and the mixing time is 2-5 h.
Typical but non-limiting mixing temperatures are 120 ℃, 125 ℃, 130 ℃, 135 ℃, 140 ℃, 145 ℃, 150 ℃, 155 ℃ or 160 ℃. Typical but non-limiting mixing times are 2h, 3h, 4h or 5 h.
As an optional implementation mode of the invention, the injection temperature is 140-170 ℃, the injection peak pressure is 30-70MPa, and the pressure maintaining pressure is 30-50 MPa.
Typical but non-limiting injection temperatures are 140 ℃, 150 ℃, 160 ℃ or 170 ℃. Typical but non-limiting injection peak pressures are 30MPa, 40MPa, 50MPa, 60MPa or 70 MPa. Typical but non-limiting dwell pressures are 30MPa, 40MPa or 50 MPa.
As an alternative embodiment of the present invention, the degreasing treatment includes a step of immersing and degreasing the green body in a degreasing solvent.
After the blank is degreased by adopting the buried burning powder in the prior art, the surface of the ceramic body is generally adhered with ceramic powder particles used by the residual buried burning powder, so that the ceramic powder particles are difficult to clean, and the appearance and the function of the atomization core are greatly influenced. And soaking the green body in a degreasing solvent for degreasing, and precipitating the organic binder through the dissolving action of the degreasing solvent. Compared with the traditional method of degreasing by adopting the buried burning powder, the method of degreasing by adopting the degreasing solvent can effectively avoid the pollution caused by the buried burning powder remained on the surface of the ceramic body.
As an alternative embodiment of the present invention, the degreasing solvent includes any one of paraffin oil, kerosene or gasoline.
As an alternative embodiment of the invention, the time of the degreasing treatment is 10-24 h. Typical but non-limiting degreasing treatment times are 10h, 12h, 14h, 16h, 18h, 20h, 22h or 24 h.
As an alternative embodiment of the present invention, the degreasing treatment further includes a drying step before sintering.
As an optional implementation mode of the invention, the sintering temperature is 850-1050 ℃, the sintering time is 10-30min, the sintering atmosphere is vacuum, and the vacuum degree is less than or equal to 10 Pa.
Typical but non-limiting sintering temperatures are 850 deg.C, 860 deg.C, 880 deg.C, 900 deg.C, 920 deg.C, 940 deg.C, 950 deg.C, 960 deg.C, 980 deg.C, 1000 deg.C, 1020 deg.C, 1040 deg.C or 1050 deg.C. Typical but non-limiting sintering times are 10min, 20min or 30 min.
According to a fourth aspect of the present invention, there is provided a ceramic atomizing core comprising the above-described porous ceramic body and an electrode.
In view of the advantages of the porous ceramic body, the ceramic atomizing core prepared by the ceramic atomizing core is continuously sucked for 500 mouths under a certain power (7.5W), the fluctuation of the average atomizing amount (TPM) is less than or equal to +/-10 percent, and the mouthfeel is not obviously pasted.
As an alternative embodiment of the invention, the electrode is a metal electrode.
According to a fifth aspect of the present invention, there is provided a method for preparing the above ceramic atomizing core, comprising the steps of:
and printing the slurry for forming the electrode on the surface of the porous ceramic body, and then calcining to obtain the ceramic atomizing core.
As an alternative embodiment of the invention, the slurry is a metal slurry, preferably a nichrome slurry.
As an optional implementation mode of the invention, the calcination temperature is 850-.
Typical but non-limiting calcination temperatures are 850 deg.C, 880 deg.C, 900 deg.C, 920 deg.C, 950 deg.C, 980 deg.C, 1000 deg.C, 1020 deg.C, 1040 deg.C or 1050 deg.C.
According to a sixth aspect of the present invention, there is provided an electronic cigarette comprising the above porous ceramic body or the above ceramic atomizing core.
In view of the advantages of the porous ceramic body or the ceramic atomizing core, the electronic cigarette comprising the porous ceramic body or the ceramic atomizing core also has the same advantages.
The present invention will be further described with reference to specific examples and comparative examples.
Example 1-example 14
Examples 1-14 each provide a glass frit having the specific composition shown in table 1.
The preparation method of the glass powder provided by each embodiment comprises the following steps:
weighing 2kg of powder according to the raw material ratio in Table 1, adding 2.5kg of pure water, and stirring for 10min to obtain CO2Fully waveAnd putting the slurry into a ball milling tank, grinding for 2h at the rotating speed of 320r/min, testing the powder granularity D50 to be 3 mu m, stopping grinding, discharging and drying to obtain mixed powder.
Putting the mixed powder into a silicon oxide crucible, preserving heat at different melting temperatures for 4h for melting, and then pouring the obtained molten glass into water for quenching to obtain glass slag;
putting the glass slag into a ball milling tank made of alumina, adding pure water according to the material-water ratio of 1:1 by weight, grinding for 2 hours at the rotating speed of 320r/min, filtering the discharged slurry by using a 300-mesh screen, and drying the slurry under the screen to obtain glass powder.
Comparative examples 1 to 2
Comparative examples 1 to 2 each provide a glass frit having a specific composition as shown in table 1, and prepared in the same manner as in examples 1 to 14.
TABLE 1
As can be seen from Table 1, the glass frits provided by the examples have softening points of 950 ℃ and 1150 ℃. While comparative examples 1 and 2 did not have softening points within 950-1150 ℃.
Example 15 example 26
Examples 15 to 26 each provide a porous ceramic material for an atomizing core using the glass frit provided in examples 2, 8 or 14, respectively, and the specific composition of the porous ceramic material for an atomizing core is shown in table 2.
In table 2, glass frit 2# corresponds to the glass frit of example 2, glass frit 8# corresponds to the glass frit of example 8, and glass frit 14# corresponds to the glass frit of example 14.
Comparative examples 3 to 6
Comparative examples 3 to 6 each provide a porous ceramic material for an atomizing core using the glass frit provided in comparative examples 1 and 2 or example 2, respectively, and the specific composition of the porous ceramic material for an atomizing core is shown in table 2.
In table 2, glass frit No. 15 corresponds to the glass frit of comparative example 1, and glass frit No. 16 corresponds to the glass frit of comparative example 2.
TABLE 2
The porous ceramic bodies made of the porous ceramic materials for the atomizing cores provided in examples 15 to 26 and comparative examples 3 to 6 were prepared by the following specific methods:
mixing the raw materials of the porous ceramic material according to the sequence of the organic binder, the aggregate and the pore-forming agent, adding each raw material, mixing for 0.5-1h, adding the next raw material, and mixing the obtained mixture at the mixing temperature of 140 ℃ for 4h to obtain an injection feed;
injection molding is carried out on the injection feed by adopting a horizontal electric injection machine, the injection temperature is 160 ℃, the injection peak pressure is 50MPa, and the pressure maintaining pressure is 30MPa, so as to obtain a green body;
and soaking the green body by using paraffin oil for 20h, removing paraffin and palm wax in the green body, drying the green body at a low temperature of 40 ℃ for 10h after soaking, sintering the green body at different sintering temperatures (shown in table 3), and preserving heat for 3h to obtain a porous ceramic body (with the size of 9 x 3.5 x 3 mm).
The ceramic atomizing core is prepared from the porous ceramic body, and the specific preparation method comprises the following steps:
on the porous ceramic bodies prepared in the embodiments and the comparative examples, the electrode is printed by using a nickel-chromium alloy paste, after the printing is finished, the electrodes are dried at the temperature of 100 ℃, then the electrodes are vacuumized and calcined in a vacuum furnace, the calcining temperature is 950 ℃, the heat preservation time is 10min, the vacuum degree is kept to be less than or equal to 10Pa in the whole process, and the ceramic atomization core is obtained, wherein the specific structure is shown in figures 2-5.
Meanwhile, the compressive strength, the porosity and the oil absorption rate of the prepared porous ceramic body are detected, and specific detection results are shown in table 3.
The compression strength test method comprises the following steps: according to the test method for the compression strength of porous ceramics GB/T1964-1996, a cube with the sample size of 20mm is tested by a universal testing machine.
Porosity test method: the test is carried out according to the test method for porosity and volume weight of porous ceramics GB/T1966-1996.
The oil absorption rate adopts a general full-automatic ceramic atomizing core oil absorption rate tester in the industry, and the test method comprises the following steps: the tobacco tar for testing is put into a thermostatic cup, a ceramic atomizing core is vertically hung, the rising displacement is set, an equipment starting button is clicked, the instrument automatically rises the tobacco tar to the position contacting the lower end of the ceramic core, and meanwhile, the weight change values of all time points in the tobacco tar climbing process are recorded and a weight change curve along with time is generated.
The size and consistency of the smoke amount adopt general equipment in the industry: the smoke concentration tester (including TPM) tests, and the testing principle of the smoke quantity (total particulate matter, TPM) is as follows: the manual smoking process is simulated by utilizing equipment, smoke exhausted after atomization of each mouth is completely absorbed through a porous-like organic material oil absorption sheet, then the weight change of the oil absorption sheet is weighed periodically (for example, every 50 mouths), and the change is divided by the corresponding number of the mouths, so that the average atomization amount in the detection time period can be obtained. Fig. 6 is a graph showing changes in the average amount of smoke in the ceramic atomizing core made of the porous ceramic material for an atomizing core provided in example 17.
TABLE 3
As can be seen from the data in Table 3, if the softening point of the glass frit is high, the sintering temperature of the ceramic needs to be increased accordingly. The softening point and the addition amount of the glass have important influences on the sintering temperature, the compressive strength, the porosity and the oil absorption rate of the porous ceramic body. The proper types and addition amounts of the added glass powder are selected, which is beneficial to realizing the balance among various properties of the porous ceramic body.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. The porous ceramic material for the atomizing core is characterized by comprising the following components in percentage by mass based on 100 percent of the mass fraction of the porous ceramic material:
40-55% of aggregate, 35-45% of pore-forming agent and 10-20% of organic binder;
wherein the aggregate comprises glass powder and SiO2Ceramic powder of said SiO-containing2The mass ratio of the ceramic powder to the glass powder is 1: (0.5-1), and the softening point of the glass powder is 950-.
2. The porous ceramic material for the atomizing core according to claim 1, wherein the glass powder comprises the following raw materials in percentage by mass, calculated as 100% of the glass powder in percentage by mass:
SiO2 60-80％，Al2O3 2-10％，Na2CO3 0-5％，Ca3(PO4)2 1-10％，MgO 1-5％，H3BO3 5-15％，TiO20-2% and ZnO 0-5%.
3. The porous ceramic material for the atomizing core according to claim 2, characterized in that the preparation method of the glass powder comprises the following steps:
(a) mixing and grinding raw materials of glass powder, then carrying out high-temperature melting, and quenching the obtained glass liquid to obtain glass slag;
(b) grinding the glass slag to obtain glass powder;
preferably, in step (a), grinding to a particle size D50 ≤ 10 μm;
preferably, in the step (a), the melting temperature is 1500-;
preferably, in step (a), the quenching is water quenching;
preferably, in step (b), the milling is carried out to a particle size D50 of 10 to 30 μm.
4. The porous ceramic material for atomizing core according to any one of claims 1 to 3, wherein the SiO-containing porous ceramic material2The ceramic powder comprises any one or the combination of at least two of diatomite, quartz sand, mullite or cordierite, and is preferably diatomite;
preferably, the pore-forming agent is graphite, and the granularity D50 of the graphite is 10-30 μm;
preferably, the organic binder comprises the following raw materials in percentage by mass, calculated by taking the organic binder as 100% in percentage by mass:
55-75% of semi-refined paraffin, 5-20% of carnauba wax and 10-30% of polypropylene.
5. A porous ceramic body, characterized in that it is made of a porous ceramic material for an atomizing core according to any one of claims 1 to 4;
the porous ceramic body has an oil absorption rate of 10-14 mg/s.
6. The porous ceramic body of claim 5, wherein the porous ceramic body has a compressive strength of 17-26 MPa;
and/or the porous ceramic body has a porosity of 62-75%.
7. The method of preparing a porous ceramic body of claim 5 or 6, comprising the steps of:
mixing the raw materials of the porous ceramic material for the atomizing core, and performing injection molding to obtain a green body;
degreasing the green body, and sintering to obtain a porous ceramic body;
preferably, the mixing temperature is 120-160 ℃, and the mixing time is 2-5 h;
preferably, the injection temperature is 140-;
preferably, the degreasing treatment comprises the step of soaking and degreasing the green body in a degreasing solvent;
preferably, the degreasing solvent comprises any one of paraffin oil, kerosene or gasoline;
preferably, the time of the degreasing treatment is 10-24 h;
preferably, the degreasing treatment is followed by a drying step before sintering;
preferably, the sintering temperature is 850-1050 ℃, the sintering time is 10-30min, the sintering atmosphere is vacuum, and the vacuum degree is less than or equal to 10 Pa.
8. A ceramic atomizing core comprising the porous ceramic body of claim 5 or 6 and an electrode;
preferably, the electrode is a metal electrode.
9. The method of making a ceramic atomizing core of claim 8, comprising the steps of:
printing the slurry for forming the electrode on the surface of the porous ceramic body, and then calcining to obtain a ceramic atomizing core;
preferably, the slurry is a metal slurry, preferably a nickel-chromium alloy slurry;
preferably, the calcination temperature is 850-1050 ℃, the heat preservation time is 10-30min, the calcination atmosphere is vacuum, and the vacuum degree is less than or equal to 10 Pa.
10. An electronic cigarette comprising the porous ceramic body of claim 5 or 6 or the ceramic atomizing core of claim 8.
Priority Applications (1)
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| CN115417690A (en) * | 2022-08-29 | 2022-12-02 | 新化县宏立磁性陶瓷有限公司 | Porous ceramic material for electronic cigarette atomization core and preparation method thereof |
| CN115819110A (en) * | 2022-12-16 | 2023-03-21 | 深圳市吉迩技术有限公司 | Metallized porous ceramic composite material and preparation method thereof |
| WO2024124643A1 (en) * | 2022-12-13 | 2024-06-20 | 深圳市吉迩技术有限公司 | High-power ceramic heating body and preparation method therefor |
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