CN115073204B - Porous ceramic, preparation method and application thereof, porous ceramic composition precursor, electronic cigarette atomization core and electronic cigarette - Google Patents

Porous ceramic, preparation method and application thereof, porous ceramic composition precursor, electronic cigarette atomization core and electronic cigarette Download PDF

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CN115073204B
CN115073204B CN202110261685.5A CN202110261685A CN115073204B CN 115073204 B CN115073204 B CN 115073204B CN 202110261685 A CN202110261685 A CN 202110261685A CN 115073204 B CN115073204 B CN 115073204B
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oxide
parts
porous ceramic
electronic cigarette
niobium
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CN115073204A (en
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陈戈
林信平
唐威
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BYD Co Ltd
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BYD Co Ltd
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    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
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Abstract

In order to solve the problem that the nickel lead falls off due to insufficient toughness of the porous ceramic atomizing core of the existing electronic cigarette, the application provides porous ceramic, which is characterized by comprising the following components in parts by weight: 45 to 98.9 parts of ceramic matrix, 0.6 to 20 parts of sintering-aid oxide, 0.0005 to 0.25 part of niobium oxide and 0.1 to 10 parts of yttrium-stabilized zirconium oxide. Meanwhile, the application also discloses application of the preparation method of the porous ceramic, a porous ceramic composition precursor for preparing the porous ceramic, an electronic cigarette atomization core and an electronic cigarette comprising the porous ceramic. The porous ceramic provided by the application is mainly applied to an electronic cigarette atomization core, has better strength and toughness, and can prevent nickel leads from shrinking and falling off on the porous ceramic during sintering.

Description

Porous ceramic, preparation method and application thereof, porous ceramic composition precursor, electronic cigarette atomization core and electronic cigarette
Technical Field
The application belongs to the technical field of electronic cigarette structures, and particularly relates to porous ceramic, a preparation method and application thereof, a porous ceramic composition precursor, an electronic cigarette atomization core and an electronic cigarette.
Background
At present, the electronic cigarette is popular in European and American areas, and the performance of the porous ceramic atomization core directly determines the taste of smoking, so that the porous ceramic atomization core is a core part of the electronic cigarette. In the process of preparing the porous ceramic of the electronic cigarette, the nickel lead and the porous ceramic are required to be sintered together, the shrinkage rate of the nickel lead during sintering is large, and if the toughness of the porous ceramic is insufficient, the nickel lead can be pulled off from the joint of ceramic blanks by shrinkage of the nickel lead, or even if the nickel lead is combined in the sintering process, the nickel lead is also subjected to subsequent falling risk, so that adverse effects are brought to the process yield and the service life. The strength and toughness of the substance formed by the conventional porous atomization core ceramic are not high, so that the strength and toughness of the sintered porous ceramic atomization core are low, the powder falling problem is caused, and the conductive metal lead is torn off from a ceramic blank due to shrinkage when the conductive metal lead is sintered together later, so that the instability of a product is finally caused. Therefore, development of an atomized core ceramic with high toughness has a great pushing effect on development of the electronic cigarette industry.
Disclosure of Invention
Aiming at the problem that the nickel lead falls off due to insufficient toughness of the porous ceramic atomization core of the existing electronic cigarette, the application provides porous ceramic, a preparation method and application thereof, a porous ceramic composition precursor, the electronic cigarette atomization core and the electronic cigarette.
The technical scheme adopted by the application for solving the technical problems is as follows:
in one aspect, the application provides a porous ceramic comprising the following components in weight:
45 to 98.9 parts of ceramic matrix, 0.6 to 20 parts of sintering-aid oxide, 0.0005 to 0.25 part of niobium oxide and 0.1 to 10 parts of yttrium-stabilized zirconium oxide.
Optionally, the porous ceramic comprises the following components in parts by weight:
58 to 97.2 parts of ceramic matrix, 1.8 to 15 parts of sintering-aid oxide, 0.01 to 0.15 part of niobium oxide and 1 to 3 parts of yttrium-stabilized zirconium oxide.
Optionally, the porous ceramic is composed of the following components in parts by weight:
45 to 98.9 parts of ceramic matrix, 0.6 to 20 parts of sintering-aid oxide, 0.0005 to 0.25 part of niobium oxide and 0.1 to 10 parts of yttrium-stabilized zirconium oxide.
Optionally, the niobium oxide includes one or more of niobium monoxide, niobium dioxide, niobium trioxide and niobium pentoxide.
Optionally, the yttrium-stabilized zirconium oxide comprises 2 to 4 mole percent yttrium oxide.
Optionally, the ceramic matrix comprises the following components in parts by weight:
10-50 parts of aluminum oxide and 35-85 parts of silicon oxide.
Optionally, the sintering-assisting oxide comprises the following components in parts by weight:
0.2 to 7 parts of magnesium oxide, 0.2 to 7 parts of calcium oxide and 0.2 to 6 parts of bismuth oxide.
In another aspect, the present application provides a method for preparing the porous ceramic as described above, comprising the following steps:
mixing a ceramic matrix, a sintering-assisting oxide, a niobium oxide and a yttrium-stabilized zirconium oxide according to the weight portion ratio, ball milling, and drying to obtain composite powder;
mixing and molding the composite powder, a pore-forming agent and a binder to obtain a blank;
sintering the green body to remove the binder and pore-forming agent to obtain the porous ceramic.
Optionally, in the ball milling process, the ceramic matrix, the burn-up oxide, the niobium oxide and the yttrium-stabilized zirconium oxide are prepared according to the following steps: 45 to 98.9 parts of ceramic matrix, 0.6 to 20 parts of sintering-assisting oxide, 0.0005 to 0.25 part of niobium oxide and 0.1 to 10 parts of yttrium-stabilized zirconium oxide are mixed together.
Optionally, during the ball milling process, the ceramic matrix, the sintering aid oxide, the niobium oxide and the yttrium-stabilized zirconium oxide are prepared according to the following steps: 58 to 97.2 parts of ceramic matrix, 1.8 to 15 parts of sintering-assisting oxide, 0.01 to 0.15 part of niobium oxide and 1 to 3 parts of yttrium-stabilized zirconium oxide are mixed in a matching way.
Optionally, the niobium oxide includes one or more of niobium monoxide, niobium dioxide, niobium trioxide and niobium pentoxide.
Optionally, the yttrium-stabilized zirconium oxide comprises 2 to 4 mole percent yttrium oxide.
In another aspect, the present application provides the use of a porous ceramic as described above in an electronic cigarette atomizing core.
In another aspect, the present application provides a porous ceramic composition precursor comprising the following components by weight:
100 parts of ceramic powder, 10-40 parts of pore-forming agent and 1-5 parts of binder;
wherein the ceramic powder has the same composition as the porous ceramic.
Optionally, the pore-forming agent comprises one or more of polymethyl methacrylate, starch, carbon powder, carbonate, nitrate, ammonium salt and wood dust;
the binder includes one or more of polyvinyl alcohol, polyethylene glycol 4000, polystyrene, polyethylene, and polypropylene.
In another aspect, the application provides an electronic cigarette atomization core, which comprises the porous ceramic and a heating body positioned on the surface of the porous ceramic.
In another aspect, the present application provides an electronic cigarette comprising an electronic cigarette atomizing core as described above.
According to the porous ceramic provided by the application, the porous ceramic is mainly applied to an electronic cigarette atomization core, in order to improve the bonding strength of the porous ceramic and a nickel lead, the inventor adds yttrium stabilized zirconium oxide on the basis of a ceramic matrix and a sintering-assisting oxide to improve the overall toughness of the porous ceramic, so as to achieve the effect of adapting to the shrinkage of the nickel lead, but the simple addition of yttrium stabilized zirconium oxide cannot completely avoid the falling-off of the nickel lead, after a large number of experiments, the inventor unexpectedly discovers that adding niobium oxide with a set relative weight on the basis of a certain amount of yttrium stabilized zirconium oxide can effectively improve the toughness of the porous ceramic, further effectively avoid the falling-off problem of the nickel lead, presumably because the zirconium oxide forms a tetragonal crystal phase in the sintering process, the stabilizing effect of yttrium element is favorable for maintaining the zirconium oxide in the tetragonal crystal phase, and under the sintering state of the ceramic system, the niobium element enters the crystal lattice of the zirconium oxide, is converted into a monoclinic phase under the action of external force to prevent the falling-off of the porous ceramic from further improving the toughness of the porous ceramic, and preventing the falling-off of the porous ceramic on the porous ceramic during sintering of the nickel lead.
Detailed Description
In order to make the technical problems, technical schemes and beneficial effects solved by the application more clear, the application is further described in detail below with reference to the embodiments. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the application.
The embodiment of the application provides porous ceramic, which comprises the following components in parts by weight:
45 to 98.9 parts of ceramic matrix, 0.6 to 20 parts of sintering-aid oxide, 0.0005 to 0.25 part of niobium oxide and 0.1 to 10 parts of yttrium-stabilized zirconium oxide.
The inventors have speculated that, because zirconium oxide with stable yttrium is added on the basis of a ceramic matrix and a sintering-assisting oxide to improve the overall toughness of the porous ceramic, the effect of adapting to the shrinkage action of the nickel lead is achieved, but simply adding yttrium-stabilized zirconium oxide cannot completely avoid the falling off of the nickel lead, after a large number of experiments, the inventors have unexpectedly found that adding niobium oxide with set relative weight on the basis of a certain amount of yttrium-stabilized zirconium oxide can effectively improve the toughness of the porous ceramic, thereby effectively avoiding the falling-off problem of the nickel lead, and presumably that the stabilizing action of yttrium element is favorable for maintaining the zirconium oxide in the tetragonal phase during the sintering process of the zirconium oxide, and under the sintering state of the ceramic system, the formed crystal structure is converted into a monoclinic phase under the action of external force to prevent the crack from expanding, thereby further improving the toughness of the porous ceramic, and further avoiding the falling off of the porous ceramic due to shrinkage on the porous ceramic during the sintering of the nickel lead.
In a preferred embodiment, the porous ceramic comprises the following components by weight:
58 to 97.2 parts of ceramic matrix, 1.8 to 15 parts of sintering-aid oxide, 0.01 to 0.15 part of niobium oxide and 1 to 3 parts of yttrium-stabilized zirconium oxide.
In some embodiments, the porous ceramic is comprised of the following weight components:
45 to 98.9 parts of ceramic matrix, 0.6 to 20 parts of sintering-aid oxide, 0.0005 to 0.25 part of niobium oxide and 0.1 to 10 parts of yttrium-stabilized zirconium oxide.
It is found through specific experiments that the addition content of the niobium oxide and the addition content of the yttrium-stabilized zirconium oxide are related to the overall strength and toughness of the porous ceramic, when the addition content of the niobium oxide and the yttrium-stabilized zirconium oxide are within the above addition ranges, the improvement amplitude of the strength and toughness of the porous ceramic is maximum, the bonding strength between the porous ceramic and a nickel lead is also maximum, which means that the niobium oxide and the yttrium-stabilized zirconium oxide have obvious mutual synergistic effect in the porous ceramic, so that the niobium oxide and the yttrium-stabilized zirconium oxide need to be at least kept at certain addition levels to realize the effect, and meanwhile, too high addition levels of any component can correspondingly cause performance degradation, in particular, when the addition levels of the niobium oxide and/or the yttrium-stabilized zirconium oxide are too low, the porous ceramic cannot realize toughening effect compared with the existing porous ceramic; when the addition amount of the niobium oxide is too high, substances which cause bonding with yttrium-stabilized zirconium oxide are too soft to affect the strength of the porous ceramic; when the addition amount of the yttrium-stabilized zirconium oxide is too high, the thermal conductivity of the whole porous ceramic system is increased, and the mouthfeel of the electronic cigarette atomization is further affected.
According to an embodiment of the application, the yttrium-stabilized zirconium oxide is yttria-stabilized zirconia having a tetragonal phase.
In some embodiments, the niobium oxide includes one or more of niobium monoxide, niobium dioxide, niobium trioxide, and niobium pentoxide.
In a preferred embodiment, the niobium oxide is selected from the group consisting of niobium pentoxide.
The niobium pentoxide is a high-valence oxide of niobium, has stable property, lower preparation difficulty and cost compared with other niobium oxides, and can be prepared by burning metallic niobium in air or dehydrating niobic acid.
Niobium monoxide: also known as "niobium dioxide", of the formula NbO or Nb 2 O 2 . Is soluble in sulfuric acid, hydrochloric acid and alkali, insoluble in water, nitric acid and ethanol, and can be prepared by reducing niobium oxychloride with magnesium metal.
Niobium dioxide: chemical formula NbO 2 . Is soluble in hot alkali solution, insoluble in inorganic acid such as water and nitric acid, and ethanol. Can be heated atThe niobium pentoxide is reduced by hydrogen under the condition to prepare the catalyst.
Niobium trioxide: chemical formula Nb 2 O 3 Can be prepared by reducing niobium pentoxide by magnesium metal.
In some embodiments, the yttrium-stabilized zirconium oxide has a specific surface area of 15-20m 2 And/g, the median particle size is 0.1-0.15um.
In some embodiments, the yttrium-stabilized zirconium oxide comprises 2 to 4 mole percent yttrium oxide.
The yttrium stable zirconium oxide forms a tetragonal phase in the sintering process, and the yttrium oxide plays a role in stabilizing the tetragonal phase and improving the mechanical property, and the effect of preventing the nickel lead from falling off is improved only to a limited extent by independently adding the yttrium oxide.
The ceramic matrix functions to form a host skeleton in the porous ceramic, and in some embodiments, the ceramic matrix includes one or more of aluminum oxide, silicon oxide, diatomaceous earth, feldspar, kaolin, montmorillonite, illite, cordierite, expanded perlite, and clay. The material has the advantages of firmness, wear resistance, high temperature resistance, wide sources and low cost, and ensures the strength and toughness of the porous ceramic when being used as a ceramic matrix.
In a preferred embodiment, the ceramic matrix comprises the following weight components:
10-50 parts of aluminum oxide and 35-85 parts of silicon oxide.
In a more preferred embodiment, the aluminum oxide and silicon oxide are added in amounts of: 18-50 parts of aluminum oxide and 40-77 parts of silicon oxide.
The aluminum oxide and the silicon oxide are adopted as ceramic matrixes, and compared with other materials, the aluminum oxide and the silicon oxide have better controllability of the purity of substances, so that the uniformity of the product quality is improved. The aluminum oxide is high-temperature ceramic, plays a role in supporting a framework, forms a low-melting-point glass phase at a crystal boundary in the sintering process of the silicon oxide, promotes sintering, and plays a role in bonding the aluminum oxide.
In some embodiments, the burn-up aid oxide comprises the following components by weight:
0.2 to 7 parts of magnesium oxide, 0.2 to 7 parts of calcium oxide and 0.2 to 6 parts of bismuth oxide.
In a preferred embodiment, the magnesium oxide, calcium oxide and bismuth oxide are added in amounts of: 0.5 to 5 parts of magnesium oxide, 0.5 to 5 parts of calcium oxide and 0.8 to 5 parts of bismuth oxide.
The magnesium oxide is added into the ceramic matrix to mainly play a role of a microstructure stabilizer, so that grains can be refined, the grain boundary energy difference is greatly reduced, the anisotropism of grain growth is weakened, and discontinuous grain growth is inhibited.
The calcium oxide and the magnesium oxide are mutually matched and are used for obtaining a compact microstructure and uniform and fine grains.
The bismuth oxide is added into the ceramic matrix to play a role of a liquid phase sintering aid, reduce the sintering temperature and improve the strength of a sintered blank.
Another embodiment of the present application provides a method for preparing the porous ceramic as described above, comprising the following operation steps:
mixing a ceramic matrix, a sintering-assisting oxide, a niobium oxide and a yttrium-stabilized zirconium oxide according to the weight portion ratio, ball milling, and drying to obtain composite powder;
mixing and molding the composite powder, a pore-forming agent and a binder to obtain a blank;
sintering the green body to remove the binder and pore-forming agent to obtain the porous ceramic.
In some embodiments, during the ball milling process, the ceramic matrix, the burn-up oxide, the niobium oxide, and the yttrium-stabilized zirconium oxide are as follows: 45 to 98.9 parts of ceramic matrix, 0.6 to 20 parts of sintering-assisting oxide, 0.0005 to 0.25 part of niobium oxide and 0.1 to 10 parts of yttrium-stabilized zirconium oxide are mixed together.
In a preferred embodiment, the ceramic matrix, the burn-up oxide, the niobium oxide and the yttrium-stabilized zirconium oxide are in accordance with: 58 to 97.2 parts of ceramic matrix, 1.8 to 15 parts of sintering-assisting oxide, 0.01 to 0.15 part of niobium oxide and 1 to 3 parts of yttrium-stabilized zirconium oxide are mixed in a matching way.
In some embodiments, the niobium oxide includes one or more of niobium monoxide, niobium dioxide, niobium trioxide, and niobium pentoxide.
In some embodiments, the yttrium-stabilized zirconium oxide comprises 2 to 4 mole percent yttrium oxide.
Specifically, taking dry press molding as an example, the preparation method of the porous ceramic comprises the following operation steps:
(1) firstly, adding water into a ball milling tank for ball milling according to the weight proportion of a ceramic matrix, a sintering-assisting oxide, a niobium oxide and a yttrium-stabilized zirconium oxide, then adding a dispersing agent and water into a sand mill for sand milling, and finally adding a pore-forming agent and a binder for stirring to form slurry for spraying;
(2) sending the slurry into a spray tower for spray drying to form spherical powder with strong fluidity for dry pressing, and then dry pressing the spherical powder to form (the oil pressure of 8MPa is used for a press with 200 tons of tonnage);
(3) sintering for 1-2 hours at 1000-1300 ℃, and polishing to obtain the final sample.
It should be noted that the dry press molding is only a preferred embodiment of the porous ceramic, and is not intended to limit the present application, and in other embodiments, those skilled in the art may use other existing molding methods to prepare the porous ceramic, such as isostatic molding, injection molding, and hot die casting.
Another embodiment of the present application provides the use of a porous ceramic as described above in an electronic cigarette atomizing core.
The electronic cigarette atomization core comprises porous ceramic, a conductive layer and a nickel lead, wherein the conductive layer is positioned on the surface of the porous ceramic, and the nickel lead is inserted into the porous ceramic and is electrically connected with the conductive layer.
When the electronic cigarette atomization core is prepared, the conductive layer is formed by conducting slurry silk screen printing, and after the nickel lead is inserted into the atomization core hole preset by the porous ceramic, the nickel lead is sintered and fixed in a reducing gas furnace, and the reducing gas is selected from ammonia gas or hydrogen gas.
The porous ceramic is applied to the electronic cigarette atomization core, so that the bonding strength of the nickel lead and the porous ceramic can be effectively improved in the preparation process, and the nickel lead is prevented from falling off in the sintering process.
Another embodiment of the present application provides a porous ceramic composition precursor comprising the following components by weight:
100 parts of ceramic powder, 10-40 parts of pore-forming agent and 1-5 parts of binder;
wherein the ceramic powder has the same composition as the porous ceramic.
The porous ceramic composition precursor may be used in the preparation of the porous ceramic.
In some embodiments, the pore-forming agent comprises one or more of polymethyl methacrylate, starch, carbon powder, carbonate, nitrate, ammonium salt, and wood dust;
the binder includes one or more of polyvinyl alcohol, polyethylene glycol 4000, polystyrene, polyethylene, and polypropylene.
In a preferred embodiment, the pore-forming agent is selected from polymethyl methacrylate or starch.
In a preferred embodiment, the binder is selected from polyvinyl alcohol or polyethylene glycol 4000.
In some embodiments, the porous ceramic composition precursor further comprises a solvent by which the ceramic powder, pore formers, and binder are mixed to facilitate granulation.
The solvent comprises water and/or ethanol.
In some embodiments, the porous ceramic composition precursor further comprises a lubricant and/or dispersant.
The lubricant serves to enhance the fluidity of the porous ceramic composition precursor; the dispersing agent ensures uniformity of the porous ceramic composition precursor.
The lubricant comprises one or more of mineral wax, microcrystalline mineral wax, fischer-Tropsch wax, white wax, ceresin wax and beeswax.
The dispersant comprises a fatty acid dispersant and/or an acrylic resin dispersant.
Another embodiment of the present application provides an electronic cigarette atomization core including the porous ceramic as described above and a heating body located on a surface of the porous ceramic.
Another embodiment of the present application provides an electronic cigarette comprising an electronic cigarette atomizing core as described above.
The application is further illustrated by the following examples.
Example 1
This example is for illustrating the porous ceramic, the electronic cigarette atomizing core and the preparation method thereof disclosed by the application.
The ingredients of the porous ceramic composition precursor were as follows:
powder: wherein 25g of alumina, 66.48g of silica, 1.5g of magnesia, 3g of calcium oxide, 2g of bismuth oxide, 0.02g of niobium pentoxide and 2g of 3mol% yttrium-stabilized zirconia are added.
Pore-forming agent: PMMA (polymethyl methacrylate) was added in 26g.
10g of PVA binder (polyvinyl alcohol) was added.
100g of water was added.
The preparation method comprises the following steps:
firstly, mixing the powder in a ball milling tank for 2 hours, discharging, drying, and then, sintering in a sintering furnace for 1 hour at 1000 ℃. And (3) after the sintered powder is crushed, adding 26g of PMMA serving as a pore-forming agent, 10g of PVA binder and 100g of water, stirring and mixing for 2 hours, performing spray drying, dry-pressing the dried powder to form a green body in the shape of an electronic cigarette atomization core, and then sintering in a furnace for heat preservation at 1150 ℃ for 1.5 hours. And (3) silk-screen printing the conductive slurry on the sintered blank, inserting a nickel lead wire into a hydrogen furnace for firing, wherein the firing temperature is 1050 ℃, and obtaining the electronic cigarette atomization core.
Example 2
This example is for illustrating the porous ceramic, the electronic cigarette atomizing core and the preparation method thereof disclosed by the application.
The ingredients of the porous ceramic composition precursor were as follows:
powder: wherein 18g of alumina, 73.48g of silica, 1.5g of magnesia, 3g of calcium oxide, 2g of bismuth oxide, 0.02g of niobium pentoxide and 2g of 3mol% yttrium-stabilized zirconia are added.
Pore-forming agent: PMMA (polymethyl methacrylate) was added in 26g.
10g of PVA binder (polyvinyl alcohol) was added.
100g of water was added.
The preparation method comprises the following steps:
firstly, mixing the powder in a ball milling tank for 2 hours, discharging, drying, and then, sintering in a sintering furnace for 1 hour at 1000 ℃. And (3) after the sintered powder is crushed, adding 26g of PMMA serving as a pore-forming agent, 10g of PVA binder and 100g of water, stirring and mixing for 2 hours, performing spray drying, dry-pressing the dried powder to form a green body in the shape of an electronic cigarette atomization core, and then sintering in a furnace for heat preservation at 1150 ℃ for 1.5 hours. And (3) silk-screen printing the conductive slurry on the sintered blank, inserting a nickel lead wire into a hydrogen furnace for firing, wherein the firing temperature is 1050 ℃, and obtaining the electronic cigarette atomization core.
Example 3
This example is for illustrating the porous ceramic, the electronic cigarette atomizing core and the preparation method thereof disclosed by the application.
The ingredients of the porous ceramic composition precursor were as follows:
powder: wherein 50g of alumina, 41.48g of silica, 1.5g of magnesia, 3g of calcium oxide, 2g of bismuth oxide, 0.02g of niobium pentoxide and 2g of 3mol% yttrium-stabilized zirconia are added.
Pore-forming agent: PMMA (polymethyl methacrylate) was added in 26g.
10g of PVA binder (polyvinyl alcohol) was added.
100g of water was added.
The preparation method comprises the following steps:
firstly, mixing the powder in a ball milling tank for 2 hours, discharging, drying, and then, sintering in a sintering furnace for 1 hour at 1000 ℃. And (3) after the sintered powder is crushed, adding 26g of PMMA serving as a pore-forming agent, 10g of PVA binder and 100g of water, stirring and mixing for 2 hours, performing spray drying, dry-pressing the dried powder to form a green body in the shape of an electronic cigarette atomization core, and then sintering at 1250 ℃ in a furnace for 1.5 hours. And (3) silk-screen printing the conductive slurry on the sintered blank, inserting a nickel lead wire into a hydrogen furnace for firing, wherein the firing temperature is 1050 ℃, and obtaining the electronic cigarette atomization core.
Example 4
This example is for illustrating the porous ceramic, the electronic cigarette atomizing core and the preparation method thereof disclosed by the application.
The ingredients of the porous ceramic composition precursor were as follows:
powder: wherein 25g of alumina, 67.49g of silica, 1.5g of magnesia, 3g of calcium oxide, 2g of bismuth oxide, 0.01g of niobium pentoxide and 1g of 3mol% yttrium-stabilized zirconia are added.
Pore-forming agent: PMMA (polymethyl methacrylate) was added in 26g.
10g of PVA binder (polyvinyl alcohol) was added.
100g of water was added.
The preparation method comprises the following steps:
firstly, mixing the powder in a ball milling tank for 2 hours, discharging, drying, and then, sintering in a sintering furnace for 1 hour at 1000 ℃. After the sintered powder is crushed, 26g of PMMA as a pore-forming agent, 10g of PVA binder and 100g of water are added, stirred and mixed for 2 hours, spray drying is carried out, the dried powder is dried and pressed into a green body in the shape of an electronic cigarette atomization core, and then the green body is fired in a furnace for heat preservation for 1.5 hours at 1180 ℃. And (3) silk-screen printing the conductive slurry on the sintered blank, inserting a nickel lead wire into a hydrogen furnace for firing, wherein the firing temperature is 1050 ℃, and obtaining the electronic cigarette atomization core.
Example 5
This example is for illustrating the porous ceramic, the electronic cigarette atomizing core and the preparation method thereof disclosed by the application.
The ingredients of the porous ceramic composition precursor were as follows:
powder: wherein 25g of alumina, 65.35g of silica, 1.5g of magnesia, 3g of calcium oxide, 2g of bismuth oxide, 0.15g of niobium pentoxide and 3g of 3mol% yttrium-stabilized zirconia are added.
Pore-forming agent: PMMA (polymethyl methacrylate) was added in 26g.
10g of PVA binder (polyvinyl alcohol) was added.
100g of water was added.
The preparation method comprises the following steps:
firstly, mixing the powder in a ball milling tank for 2 hours, discharging, drying, and then, sintering in a sintering furnace for 1 hour at 1000 ℃. And (3) after the sintered powder is crushed, adding 26g of PMMA serving as a pore-forming agent, 10g of PVA binder and 100g of water, stirring and mixing for 2 hours, performing spray drying, dry-pressing the dried powder to form a green body in the shape of an electronic cigarette atomization core, and then sintering in a furnace for 1.5 hours at 1120 ℃. And (3) silk-screen printing the conductive slurry on the sintered blank, inserting a nickel lead wire into a hydrogen furnace for firing, wherein the firing temperature is 1050 ℃, and obtaining the electronic cigarette atomization core.
Comparative example 1
This comparative example is used for comparative illustration of the porous ceramic, the electronic cigarette atomizing core and the preparation method thereof disclosed by the application.
The ingredients of the porous ceramic composition precursor were as follows:
powder: wherein 25g of alumina, 68.5g of silica, 1.5g of magnesia, 3g of calcium oxide and 2g of bismuth oxide are added.
Pore-forming agent: PMMA (polymethyl methacrylate) was added in 26g.
10g of PVA binder (polyvinyl alcohol) was added.
100g of water was added.
The preparation method comprises the following steps:
firstly, mixing the powder in a ball milling tank for 2 hours, discharging, drying, and then, sintering in a sintering furnace for 1 hour at 1000 ℃. And (3) after the sintered powder is crushed, adding 26g of PMMA serving as a pore-forming agent, 10g of PVA binder and 100g of water, stirring and mixing for 2 hours, performing spray drying, dry-pressing the dried powder to form a green body in the shape of an electronic cigarette atomization core, and then sintering in a furnace at 1200 ℃ for 1.5 hours. And (3) silk-screen printing the conductive slurry on the sintered blank, inserting a nickel lead wire into a hydrogen furnace for firing, wherein the firing temperature is 1050 ℃, and obtaining the electronic cigarette atomization core.
Comparative example 2
This comparative example is used for comparative illustration of the porous ceramic, the electronic cigarette atomizing core and the preparation method thereof disclosed by the application.
The ingredients of the porous ceramic composition precursor were as follows:
powder: wherein 25g of alumina was added, 66.5g of silica was added, 1.5g of magnesia was added, 3g of calcium oxide was added, 2g of bismuth oxide was added, and 2g of 3mol% yttrium-stabilized zirconia was added.
Pore-forming agent: PMMA (polymethyl methacrylate) was added in 26g.
10g of PVA binder (polyvinyl alcohol) was added.
100g of water was added.
The preparation method comprises the following steps:
firstly, mixing the powder in a ball milling tank for 2 hours, discharging, drying, and then, sintering in a sintering furnace for 1 hour at 1000 ℃. And (3) after the sintered powder is crushed, adding 26g of PMMA serving as a pore-forming agent, 10g of PVA binder and 100g of water, stirring and mixing for 2 hours, performing spray drying, dry-pressing the dried powder to form a green body in the shape of an electronic cigarette atomization core, and then sintering in a furnace for heat preservation at 1150 ℃ for 1.5 hours. And (3) silk-screen printing the conductive slurry on the sintered blank, inserting a nickel lead wire into a hydrogen furnace for firing, wherein the firing temperature is 1050 ℃, and obtaining the electronic cigarette atomization core.
Comparative example 3
This comparative example is used for comparative illustration of the porous ceramic, the electronic cigarette atomizing core and the preparation method thereof disclosed by the application.
The ingredients of the porous ceramic composition precursor were as follows:
powder: wherein 25g of alumina, 66.5g of silica, 1.5g of magnesia, 3g of calcium oxide, 2g of bismuth oxide and 0.02g of niobium pentoxide are added.
Pore-forming agent: PMMA (polymethyl methacrylate) was added in 26g.
10g of PVA binder (polyvinyl alcohol) was added.
100g of water was added.
The preparation method comprises the following steps:
firstly, mixing the powder in a ball milling tank for 2 hours, discharging, drying, and then, sintering in a sintering furnace for 1 hour at 1000 ℃. And (3) after the sintered powder is crushed, adding 26g of PMMA serving as a pore-forming agent, 10g of PVA binder and 100g of water, stirring and mixing for 2 hours, performing spray drying, dry-pressing the dried powder to form a green body in the shape of an electronic cigarette atomization core, and then sintering in a furnace for heat preservation at 1170 ℃ for 1.5 hours. And (3) silk-screen printing the conductive slurry on the sintered blank, inserting a nickel lead wire into a hydrogen furnace for firing, wherein the firing temperature is 1050 ℃, and obtaining the electronic cigarette atomization core.
Comparative example 4
This comparative example is used for comparative illustration of the porous ceramic, the electronic cigarette atomizing core and the preparation method thereof disclosed by the application.
The ingredients of the porous ceramic composition precursor were as follows:
powder: wherein 25g of alumina, 66.5g of silica, 1.5g of magnesia, 3g of calcium oxide, 2g of bismuth oxide, 0.4g of niobium pentoxide and 2g of 3mol% yttrium-stabilized zirconia are added.
Pore-forming agent: PMMA (polymethyl methacrylate) was added in 26g.
10g of PVA binder (polyvinyl alcohol) was added.
100g of water was added.
The preparation method comprises the following steps:
firstly, mixing the powder in a ball milling tank for 2 hours, discharging, drying, and then, sintering in a sintering furnace for 1 hour at 1000 ℃. And (3) after the sintered powder is crushed, adding 26g of PMMA serving as a pore-forming agent, 10g of PVA binder and 100g of water, stirring and mixing for 2 hours, performing spray drying, dry-pressing the dried powder to form a green body in the shape of an electronic cigarette atomization core, and then sintering in a furnace to preserve heat for 1.5 hours at 1140 ℃. And (3) silk-screen printing the conductive slurry on the sintered blank, inserting a nickel lead wire into a hydrogen furnace for firing, wherein the firing temperature is 1050 ℃, and obtaining the electronic cigarette atomization core.
Comparative example 5
This comparative example is used for comparative illustration of the porous ceramic, the electronic cigarette atomizing core and the preparation method thereof disclosed by the application.
The ingredients of the porous ceramic composition precursor were as follows:
powder: wherein 25g of alumina, 66.5g of silica, 1.5g of magnesia, 3g of calcium oxide, 2g of bismuth oxide, 0.02g of niobium pentoxide and 12g of 3mol% yttrium-stabilized zirconia are added.
Pore-forming agent: PMMA (polymethyl methacrylate) was added in 26g.
10g of PVA binder (polyvinyl alcohol) was added.
100g of water was added.
The preparation method comprises the following steps:
firstly, mixing the powder in a ball milling tank for 2 hours, discharging, drying, and then, sintering in a sintering furnace for 1 hour at 1000 ℃. And (3) after the sintered powder is crushed, adding 26g of PMMA serving as a pore-forming agent, 10g of PVA binder and 100g of water, stirring and mixing for 2 hours, performing spray drying, dry-pressing the dried powder to form a green body in the shape of an electronic cigarette atomization core, and then sintering the green body in a furnace to preserve heat for 1.5 hours at 1080 ℃. And (3) silk-screen printing the conductive slurry on the sintered blank, inserting a nickel lead wire into a hydrogen furnace for firing, wherein the firing temperature is 1050 ℃, and obtaining the electronic cigarette atomization core.
Comparative example 6
This comparative example is used for comparative illustration of the porous ceramic, the electronic cigarette atomizing core and the preparation method thereof disclosed by the application.
The ingredients of the porous ceramic composition precursor were as follows:
powder: wherein 25g of alumina, 66.48g of silica, 1.5g of magnesia, 3g of calcium oxide, 2g of bismuth oxide, 0.02g of niobium pentoxide and 2g of pure zirconia are added.
Pore-forming agent: PMMA (polymethyl methacrylate) was added in 26g.
10g of PVA binder (polyvinyl alcohol) was added.
100g of water was added.
The preparation method comprises the following steps:
firstly, mixing the powder in a ball milling tank for 2 hours, discharging, drying, and then, sintering in a sintering furnace for 1 hour at 1000 ℃. And (3) after the sintered powder is crushed, adding 26g of PMMA serving as a pore-forming agent, 10g of PVA binder and 100g of water, stirring and mixing for 2 hours, performing spray drying, dry-pressing the dried powder to form a green body in the shape of an electronic cigarette atomization core, and then sintering in a furnace for heat preservation at 1150 ℃ for 1.5 hours. And (3) silk-screen printing the conductive slurry on the sintered blank, inserting a nickel lead wire into a hydrogen furnace for firing, wherein the firing temperature is 1050 ℃, and obtaining the electronic cigarette atomization core.
Performance testing
The following performance tests were performed on the electronic cigarette atomizing cores prepared in the above examples 1 to 5 and comparative examples 1 to 6:
thermal conductivity test: the thermal conductivity of the e-aerosolized core was tested using a thermal conductivity meter in accordance with the manner of standard ASTM 518.
Intensity test: the strength of the e-cig aerosol core was tested in accordance with standard GB/T6569-86 using a universal testing machine.
Drawing force test: and fixing the electronic cigarette atomization core, fixing a nickel lead through a tension meter, pulling the nickel lead from the electronic cigarette atomization core, and recording the drawing force.
The test results obtained are filled in Table 1.
TABLE 1
As can be seen from the test results of comparative examples 1 to 5 and comparative examples 1 to 3, the co-addition of niobium pentoxide and yttrium-stabilized zirconia can effectively improve the material strength and toughness of the porous ceramic, and further effectively improve the bonding strength between the porous ceramic and the nickel lead wire, and avoid the falling-off of the nickel lead wire, compared with the single addition of niobium pentoxide and yttrium-stabilized zirconia.
The test results of comparative examples 1 to 5 and comparative examples 4 and 5 show that the addition amount of niobium pentoxide and yttrium-stabilized zirconia can play a good role in improving the performance of the porous ceramic when the addition amount is controlled within a certain range, and the excessive niobium pentoxide can cause the strength of the porous ceramic to be reduced; however, the excessive yttrium-stabilized zirconia leads to an increase in the thermal conductivity of the porous ceramic, which is unfavorable for the application of the porous ceramic as an electronic cigarette atomizing core, and it is noted that the thermal conductivity of the porous ceramic used as the electronic cigarette atomizing core must be within 1.5W/(mk) to meet the requirements, and the thermal conductivity is too large, so that the porous ceramic has a burnt smell during smoking, and the taste of the porous ceramic is affected.
As can be seen from the test results of comparative examples 1 and 6, yttrium has a better stabilizing effect on zirconia, which is beneficial to improving the strength of the porous ceramics.
The foregoing description of the preferred embodiments of the application is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the application.

Claims (14)

1. The electronic cigarette atomization core is characterized by comprising porous ceramic and a heating body positioned on the surface of the porous ceramic, wherein the porous ceramic comprises the following components in parts by weight:
45 to 98.9 parts of ceramic matrix, 0.6 to 20 parts of sintering-assisting oxide, 0.0005 to 0.25 part of niobium oxide and 0.1 to 10 parts of yttrium-stabilized zirconium oxide;
the ceramic matrix comprises the following components in parts by weight:
10-50 parts of aluminum oxide and 35-85 parts of silicon oxide.
2. The electronic vaping wick of claim 1, wherein the porous ceramic comprises the following components by weight:
58 to 97.2 parts of ceramic matrix, 1.8 to 15 parts of sintering-aid oxide, 0.01 to 0.15 part of niobium oxide and 1 to 3 parts of yttrium-stabilized zirconium oxide.
3. The electronic cigarette atomizing core of claim 1, wherein the porous ceramic is comprised of the following components by weight:
45 to 98.9 parts of ceramic matrix, 0.6 to 20 parts of sintering-aid oxide, 0.0005 to 0.25 part of niobium oxide and 0.1 to 10 parts of yttrium-stabilized zirconium oxide.
4. The electronic vaping core of claim 1, wherein the niobium oxide includes one or more of niobium monoxide, niobium dioxide, niobium trioxide, and niobium pentoxide.
5. The electronic cigarette atomizing core of claim 1, wherein the yttrium-stabilized zirconium oxide comprises 2 to 4mol% yttrium oxide, based on the yttrium-stabilized zirconium oxide.
6. The electronic cigarette atomizing core of claim 5, wherein the burn-aid oxide comprises the following components in weight:
0.2 to 7 parts of magnesium oxide, 0.2 to 7 parts of calcium oxide and 0.2 to 6 parts of bismuth oxide.
7. The method for preparing an electronic cigarette atomizing core according to any one of claims 1 to 6, wherein the method for preparing the porous ceramic comprises the following steps:
mixing a ceramic matrix, a sintering-assisting oxide, a niobium oxide and a yttrium-stabilized zirconium oxide according to the weight portion ratio, ball milling, and drying to obtain composite powder;
mixing and molding the composite powder, a pore-forming agent and a binder to obtain a blank;
sintering the green body to remove the binder and pore-forming agent to obtain the porous ceramic.
8. The method for preparing an electronic cigarette atomizing core according to claim 7, wherein during the ball milling, the ceramic matrix, the burn-aid oxide, the niobium oxide and the yttrium-stabilized zirconium oxide are prepared by the following steps: 45 to 98.9 parts of ceramic matrix, 0.6 to 20 parts of sintering-assisting oxide, 0.0005 to 0.25 part of niobium oxide and 0.1 to 10 parts of yttrium-stabilized zirconium oxide are mixed together.
9. The method for preparing an electronic cigarette atomizing core according to claim 8, wherein in the ball milling process, a ceramic matrix, a sintering aid oxide, a niobium oxide and a yttrium-stabilized zirconium oxide are prepared according to the following steps: 58 to 97.2 parts of ceramic matrix, 1.8 to 15 parts of sintering-assisting oxide, 0.01 to 0.15 part of niobium oxide and 1 to 3 parts of yttrium-stabilized zirconium oxide are mixed in a matching way.
10. The method of manufacturing an electronic cigarette atomizing core according to claim 7, wherein the niobium oxide includes one or more of niobium monoxide, niobium dioxide, niobium trioxide and niobium pentoxide.
11. The method of preparing an e-cig atomizing core according to claim 7, wherein the yttrium-stabilized zirconium oxide comprises 2 to 4mol% yttrium oxide.
12. A porous ceramic composition precursor comprising the following components by weight:
100 parts of ceramic powder, 10-40 parts of pore-forming agent and 1-5 parts of binder;
wherein the ceramic powder has the same composition as the porous ceramic of the electronic cigarette atomizing core according to any one of claims 1 to 6.
13. The porous ceramic composition precursor according to claim 12, wherein the pore-forming agent comprises one or more of polymethyl methacrylate, starch, carbon powder, carbonate, nitrate, ammonium salt, and wood dust;
the binder includes one or more of polyvinyl alcohol, polyethylene glycol 4000, polystyrene, polyethylene, and polypropylene.
14. An electronic cigarette, characterized by comprising the electronic cigarette atomization core according to any one of claims 1 to 6.
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