WO2022193611A1 - 一种碱式多孔陶瓷基体及其制备方法、电子烟雾化芯和电子烟 - Google Patents

一种碱式多孔陶瓷基体及其制备方法、电子烟雾化芯和电子烟 Download PDF

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WO2022193611A1
WO2022193611A1 PCT/CN2021/120903 CN2021120903W WO2022193611A1 WO 2022193611 A1 WO2022193611 A1 WO 2022193611A1 CN 2021120903 W CN2021120903 W CN 2021120903W WO 2022193611 A1 WO2022193611 A1 WO 2022193611A1
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Prior art keywords
oxide
porous ceramic
parts
basic porous
electronic cigarette
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PCT/CN2021/120903
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English (en)
French (fr)
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陈戈
林信平
唐威
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比亚迪精密制造有限公司
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Priority to EP21931186.7A priority Critical patent/EP4292997A1/en
Publication of WO2022193611A1 publication Critical patent/WO2022193611A1/zh
Priority to US18/467,704 priority patent/US20240002294A1/en

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    • C04B38/06Porous 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
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    • AHUMAN NECESSITIES
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    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
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Definitions

  • the disclosure belongs to the technical field of electronic cigarette structures, and in particular relates to a basic porous ceramic substrate and a preparation method thereof, an electronic cigarette core and an electronic cigarette.
  • a heating body needs to be arranged on the porous ceramic substrate, and the heating body can be arranged on the porous ceramic substrate by burying a metal wire in the porous ceramic substrate, or by silk-screen printing on the porous ceramic substrate.
  • the present disclosure provides a basic porous ceramic substrate and a preparation method thereof, an electronic cigarette core and an electronic cigarette.
  • the present disclosure provides a basic porous ceramic substrate, based on the total weight of the basic porous ceramic substrate, comprising:
  • the content of the alkali metal oxide in the basic porous ceramic matrix is 1.6-12 parts
  • the content of the niobium oxide is 0.01-0.15 parts
  • the content of the yttrium-stabilized zirconium oxide is 1 to 3 servings.
  • the alkali metal oxide includes 0.5-8 parts of sodium oxide and 0.5-7 parts of potassium oxide.
  • the niobium oxide includes niobium pentoxide.
  • the yttrium-stabilized zirconium oxide has a specific surface area of 15-20 m 2 /g, and a median particle size of 0.1-0.15 ⁇ m.
  • the oxide sintering aid includes the following weight components:
  • the present disclosure provides the above-mentioned preparation method of basic porous ceramic matrix, comprising the following operation steps:
  • the ceramic powder, oxide sintering aid, alkali metal oxide, niobium oxide and yttrium-stabilized zirconium oxide are mixed in proportion by weight, ball-milled, and dried to obtain composite powder;
  • the green body is sintered to remove the binder and the pore-forming agent to obtain a basic porous ceramic matrix.
  • the present disclosure provides a basic porous ceramic substrate prepared by the above method.
  • the present disclosure provides an electronic cigarette wick, comprising the basic porous ceramic substrate as described above and a conductive layer on the surface of the basic porous ceramic substrate.
  • the present disclosure provides an electronic cigarette, including the electronic cigarette wick as described above.
  • the structural strength of the porous ceramic body is ensured, the shrinkage of the electrode lead during sintering is prevented and the ceramic substrate is prevented from falling off, and on the other hand, the bonding performance between the ceramic substrate and the printed conductive coating is improved. stronger.
  • Embodiments of the present disclosure provide a basic porous ceramic substrate, which, based on the total weight of the basic porous ceramic substrate, includes:
  • the inventor of the present disclosure accidentally found in the course of experiments that alkali metal oxides, niobium oxides and yttrium-stabilized zirconium oxides are used together in the preparation of the ceramic matrix of the ceramic atomizing core, and the prepared porous ceramic matrix has a
  • the toughness and strength of the ceramic matrix has been improved, but on the other hand, when the conductive coating is printed on the ceramic matrix by screen printing to obtain the conductive layer by sintering, the bonding strength of the ceramic matrix and the conductive layer has a certain improvement. .
  • the content of the alkali metal oxide is 1.6-12 parts
  • the content of the niobium oxide is 0.01-0.15 parts
  • the content of the yttrium-stabilized zirconium oxide is 1-3 parts.
  • the yttrium-stabilized zirconium oxide is yttria-stabilized zirconia with a tetragonal phase.
  • the alkali metal oxide includes the following weight components:
  • the addition amounts of sodium oxide and potassium oxide are: 0.8-7 parts of sodium oxide and 0.8-5 parts of potassium oxide.
  • the niobium oxide includes one or more of niobium monoxide, niobium dioxide, niobium trioxide, and niobium pentoxide.
  • the niobium oxide is selected from niobium pentoxide.
  • Niobium pentoxide is a high-valence oxide of niobium, with stable properties, lower preparation difficulty and cost than other niobium oxides, and can be prepared by burning metal niobium in air or dehydrating niobic acid.
  • the yttrium-stabilized zirconium oxide has a specific surface area of 15-20 m 2 /g and a median particle size of 0.1-0.15 ⁇ m.
  • the yttrium-stabilized zirconium oxide includes 2-4 mol% yttrium oxide.
  • the yttrium-stabilized zirconium oxide forms a tetragonal crystal phase during the sintering process, and the yttrium oxide plays the role of stabilizing its tetragonal crystal phase and improves the mechanical properties. It should be noted that adding yttrium oxide alone can prevent the electrode leads from falling off. In the technical solution of the present disclosure, the yttrium-stabilized zirconium oxide can achieve the material toughness required to prevent the electrode lead from falling off only after adding niobium oxide.
  • the ceramic powder plays the role of forming the main framework in the basic porous ceramic matrix.
  • the ceramic powder includes aluminum oxide, silicon oxide, diatomaceous earth, feldspar, and kaolin.
  • the above substances have the advantages of firmness, wear resistance, high temperature resistance, wide source and low cost. When used as ceramic powders, the strength and toughness of porous ceramics are ensured.
  • the ceramic powder includes the following weight components:
  • the addition amounts of aluminum oxide and silicon oxide are: 18-50 parts of aluminum oxide and 40-77 parts of silicon oxide.
  • aluminum oxide and silicon oxide as ceramic powder, compared with other materials, its material purity has better controllability, which is conducive to improving the consistency of product quality.
  • aluminum oxide is a high-temperature ceramic, which plays the role of skeleton support, and silicon oxide forms a low-melting glass phase at the grain boundary during the sintering process, which promotes sintering and plays a role in bonding the aluminum oxide.
  • the oxide sintering aid includes the following components by weight:
  • the addition amounts of magnesium oxide and calcium oxide are: 0.5-5 parts of magnesium oxide and 0.5-5 parts of calcium oxide.
  • the addition of the magnesium oxide to the ceramic powder mainly acts as a microstructure stabilizer, which can refine the grains, greatly reduce the energy difference between grain boundaries, weaken the anisotropy of grain growth, and inhibit discontinuity. grain growth.
  • the calcium oxide and the magnesium oxide cooperate with each other to obtain a dense microstructure and uniform and fine grains.
  • Another embodiment of the present disclosure provides the above-mentioned preparation method of the basic porous ceramic matrix, comprising the following operation steps:
  • the ceramic powder, oxide sintering aid, alkali metal oxide, niobium oxide and yttrium-stabilized zirconium oxide are mixed in proportion by weight, ball-milled, and dried to obtain composite powder;
  • the green body is sintered to remove the binder and the pore-forming agent to obtain a basic porous ceramic matrix.
  • the preparation method of the basic porous ceramic matrix includes the following operation steps:
  • the ceramic powder, oxide sintering aids, alkali metal oxides, niobium oxides and yttrium-stabilized zirconium oxides are ball-milled with water in the ball mill tank according to the weight ratio, and then the dispersant and water are added to the sand mill. Sand grinding, and finally add pore-forming agent and binder to stir to form a slurry for spraying;
  • the slurry is sent to the spray tower for spray drying to form spherical powder with strong fluidity for dry pressing, and then the spherical powder is dry-pressed (the press with a tonnage of 200 tons uses an oil pressure of 8MPa);
  • the basic porous ceramic substrate can be prepared by other existing molding methods, such as isostatic pressing molding, injection molding, hot die casting molding and other molding methods.
  • Another embodiment of the present disclosure provides the basic porous ceramic matrix prepared by the above method.
  • the electronic cigarette vaporization core includes a basic porous ceramic base, a conductive layer and electrode leads, the conductive layer is located on the surface of the basic porous ceramic base, so The electrode leads are inserted into the basic porous ceramic base and are electrically connected to the conductive layer; the conductive layer is obtained by silk-screening the conductive paste on the surface of the basic porous ceramic base and then sintering.
  • the conductive layer is formed by screen printing with conductive paste, and the electrode lead is inserted into the predetermined atomizing core hole of the basic porous ceramic substrate, and then sintered in a reducing gas furnace
  • the fixed, reducing gas is selected from ammonia or hydrogen.
  • Applying the basic porous ceramic substrate to the electronic cigarette wick can effectively improve the bonding strength of the electrode lead and the basic porous ceramic substrate during the preparation process, prevent the electrode lead from falling off during the sintering process, and at the same time ensure the The effect of screen printing improves the bonding force of the conductive layer.
  • Another embodiment of the present disclosure provides an electronic cigarette, including the electronic cigarette wick as described above.
  • a basic porous ceramic matrix composition is provided, and the ingredients are as follows:
  • Powder Add 25g of alumina, 66.48g of silicon oxide, 1.5g of magnesium oxide, 3g of calcium oxide, 1g of sodium oxide, 1g of potassium oxide, 0.02g of niobium pentoxide, 3mol% yttrium-stabilized oxide Zirconium was added 2g.
  • Pore-forming agent PMMA (polymethyl methacrylate) was added in 26 g.
  • PVA binder polyvinyl alcohol
  • the specific preparation method is as follows:
  • the powder is mixed in the ball mill for 2 hours. After the material is discharged and dried, it is fired in a sintering furnace at 1000°C for 1 hour. After the fired powder is crushed, add 26 g of PMMA as a pore-forming agent, 10 g of PVA binder and 100 g of water, stir and mix for 2 hours, spray-dry, and dry-press the dried powder into a green body in the shape of an electronic cigarette core. , and then fired into the furnace at 1140°C for 1.5h. The sintered green body is screen-printed with conductive paste and inserted into the electrode leads, and is fired in a hydrogen furnace at a firing temperature of 1050° C. to obtain an electronic cigarette core.
  • a basic porous ceramic matrix composition is provided, and the ingredients are as follows:
  • Powder Add 18g of alumina, 73.48g of silicon oxide, 1.5g of magnesium oxide, 3g of calcium oxide, 0.5g of sodium oxide, 0.5g of potassium oxide, 0.02g of niobium pentoxide, 3 mol% yttrium to stabilize 2 g of zirconia was added.
  • Pore-forming agent PMMA (polymethyl methacrylate) was added in 26 g.
  • PVA binder polyvinyl alcohol
  • the specific preparation method is as follows:
  • the powder is mixed in the ball mill for 2 hours. After the material is discharged and dried, it is fired in a sintering furnace at 1000°C for 1 hour. After the fired powder is crushed, add 26 g of PMMA as a pore-forming agent, 10 g of PVA binder and 100 g of water, stir and mix for 2 hours, spray-dry, and dry-press the dried powder into a green body in the shape of an electronic cigarette core. , and then fired into the furnace at 1140°C for 1.5h. The sintered green body is screen-printed with conductive paste and inserted into the electrode leads, and is fired in a hydrogen furnace at a firing temperature of 1050° C. to obtain an electronic cigarette core.
  • a basic porous ceramic matrix composition is provided, and the ingredients are as follows:
  • Powder Add 50g of alumina, 41.48g of silicon oxide, 1.5g of magnesium oxide, 3g of calcium oxide, 2g of sodium oxide, 2g of potassium oxide, 0.02g of niobium pentoxide, 3mol% yttrium-stabilized oxide Zirconium was added 2g.
  • Pore-forming agent PMMA (polymethyl methacrylate) was added in 26 g.
  • PVA binder polyvinyl alcohol
  • the specific preparation method is as follows:
  • the powder is mixed in the ball mill for 2 hours. After the material is discharged and dried, it is fired in a sintering furnace at 1000°C for 1 hour. After the fired powder is crushed, add 26 g of PMMA as a pore-forming agent, 10 g of PVA binder and 100 g of water, stir and mix for 2 hours, spray-dry, and dry-press the dried powder into a green body in the shape of an electronic cigarette core. , and then fired into the furnace at 1235°C for 1.5h. The sintered green body is screen-printed with conductive paste and inserted into the electrode leads, and is fired in a hydrogen furnace at a firing temperature of 1050° C. to obtain an electronic cigarette core.
  • a basic porous ceramic matrix composition is provided, and the ingredients are as follows:
  • Powder Add 25g of alumina, 67.49g of silicon oxide, 1.5g of magnesium oxide, 3g of calcium oxide, 5g of sodium oxide, 5g of potassium oxide, 0.01g of niobium pentoxide, 3mol% yttrium-stabilized oxide Zirconium was added by 1 g.
  • Pore-forming agent PMMA (polymethyl methacrylate) was added in 26 g.
  • PVA binder polyvinyl alcohol
  • the specific preparation method is as follows:
  • the powder is mixed in the ball mill for 2 hours. After the material is discharged and dried, it is fired in a sintering furnace at 1000°C for 1 hour. After the fired powder is crushed, add 26 g of PMMA as a pore-forming agent, 10 g of PVA binder and 100 g of water, stir and mix for 2 hours, spray-dry, and dry-press the dried powder into a green body in the shape of an electronic cigarette core. , and then fired into the furnace at 1170°C for 1.5h. The sintered green body is screen-printed with conductive paste and inserted into the electrode leads, and is fired in a hydrogen furnace at a firing temperature of 1050° C. to obtain an electronic cigarette core.
  • a basic porous ceramic matrix composition is provided, and the ingredients are as follows:
  • Powder Add 25g of alumina, 65.35g of silicon oxide, 1.5g of magnesium oxide, 3g of calcium oxide, 7g of sodium oxide, 8g of potassium oxide, 0.15g of niobium pentoxide, 3mol% yttrium-stabilized oxide Zirconium was added in 3 g.
  • Pore-forming agent PMMA (polymethyl methacrylate) was added in 26 g.
  • PVA binder polyvinyl alcohol
  • the specific preparation method is as follows:
  • the powder is mixed in the ball mill for 2 hours. After the material is discharged and dried, it is fired in a sintering furnace at 1000°C for 1 hour. After the fired powder is crushed, add 26 g of PMMA as a pore-forming agent, 10 g of PVA binder and 100 g of water, stir and mix for 2 hours, spray-dry, and dry-press the dried powder into a green body in the shape of an electronic cigarette core. , and then fired into the furnace at 1100°C for 1.5h. The sintered green body is screen-printed with conductive paste and inserted into the electrode leads, and then fired in a hydrogen furnace at a firing temperature of 1050°C to obtain an electronic cigarette core.
  • a porous ceramic matrix composition is provided, and the ingredients are as follows:
  • Powder Add 25g of alumina, 66.48g of silicon oxide, 1.5g of magnesium oxide, 3g of calcium oxide, 2g of bismuth oxide, 0.02g of niobium pentoxide, and 2g of 3mol% yttrium-stabilized zirconia.
  • Pore-forming agent PMMA (polymethyl methacrylate) was added in 26 g.
  • PVA binder polyvinyl alcohol
  • the specific preparation method is as follows:
  • the powder is mixed in the ball mill for 2 hours. After the material is discharged and dried, it is fired in a sintering furnace at 1000°C for 1 hour. After the fired powder is crushed, add 26 g of PMMA as a pore-forming agent, 10 g of PVA binder and 100 g of water, stir and mix for 2 hours, spray-dry, and dry-press the dried powder into a green body in the shape of an electronic cigarette core. , and then fired into the furnace at 1070°C for 1.5h. The sintered green body is screen-printed with conductive paste and inserted into the electrode leads, and is fired in a hydrogen furnace at a firing temperature of 1050° C. to obtain an electronic cigarette core.
  • a porous ceramic matrix composition is provided, and the ingredients are as follows:
  • Powder Add 25g of alumina, 66.48g of silicon oxide, 1.5g of magnesium oxide, 3g of calcium oxide, 1g of sodium oxide, 1g of potassium oxide, and 2g of 3mol% yttrium-stabilized zirconia.
  • Pore-forming agent PMMA (polymethyl methacrylate) was added in 26 g.
  • PVA binder polyvinyl alcohol
  • the specific preparation method is as follows:
  • the powder is mixed in the ball mill for 2 hours. After the material is discharged and dried, it is fired in a sintering furnace at 1000°C for 1 hour. After the fired powder is crushed, add 26 g of PMMA as a pore-forming agent, 10 g of PVA binder and 100 g of water, stir and mix for 2 hours, spray-dry, and dry-press the dried powder into a green body in the shape of an electronic cigarette core. , and then fired into the furnace at 1140°C for 1.5h. The sintered green body is screen-printed with conductive paste and inserted into the electrode leads, and is fired in a hydrogen furnace at a firing temperature of 1050° C. to obtain an electronic cigarette core.
  • a porous ceramic matrix composition is provided, and the ingredients are as follows:
  • Powder Add 25g of alumina, 66.48g of silicon oxide, 1.5g of magnesium oxide, 3g of calcium oxide, 1g of sodium oxide, 1g of potassium oxide, and 0.02g of niobium pentoxide.
  • Pore-forming agent PMMA (polymethyl methacrylate) was added in 26 g.
  • PVA binder polyvinyl alcohol
  • the specific preparation method is as follows:
  • the powder is mixed in the ball mill for 2 hours. After the material is discharged and dried, it is fired in a sintering furnace at 1000°C for 1 hour. After the fired powder is crushed, add 26 g of PMMA as a pore-forming agent, 10 g of PVA binder and 100 g of water, stir and mix for 2 hours, spray-dry, and dry-press the dried powder into a green body in the shape of an electronic cigarette core. , and then fired into the furnace at 1170°C for 1.5h. The sintered green body is screen-printed with conductive paste and inserted into the electrode leads, and is fired in a hydrogen furnace at a firing temperature of 1050° C. to obtain an electronic cigarette core.
  • Thermal conductivity test According to the standard ASTM518 method, use a thermal conductivity meter to test the thermal conductivity of the electronic cigarette core.
  • Pulling force test Fix the vape core, fix the electrode lead with a tension gauge, pull the electrode lead off the vape core, and record the pulling force used.
  • the bonding strength test of the ceramic substrate and the conductive layer heat the electronic cigarette core at 60 degrees for two seconds, and then place it at 10 degrees and cool it for 5 seconds.
  • As a thermal shock test when the conductive layer falls off, record the electronic cigarette Number of thermal shock tests for aerosol cores.

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Abstract

一种碱式多孔陶瓷基体,以碱式多孔陶瓷基体的总重量为基准,包括:陶瓷粉体45-98.1份、氧化物助烧剂0.4-14份、碱金属氧化物1-15份、铌氧化物0.0005-0.25份和钇稳定的锆氧化物0.1-10份。一种碱式多孔陶瓷基体的制备方法、包括上述碱式多孔陶瓷基体的电子烟雾化芯和电子烟。

Description

一种碱式多孔陶瓷基体及其制备方法、电子烟雾化芯和电子烟
本公开要求于2021年03月19日提交中国专利局,申请号为202110297287.9,申请名称为“一种碱式多孔陶瓷基体及其制备方法、电子烟雾化芯和电子烟”的中国专利申请的优先权,其全部内容通过引用结合在本公开中。
技术领域
本公开属于电子烟结构技术领域,具体涉及一种碱式多孔陶瓷基体及其制备方法、电子烟雾化芯和电子烟。
背景技术
现有制备电子烟的过程中,需要在多孔陶瓷基体上设置加热体,多孔陶瓷基体上设置加热体的方式可以是将金属丝埋设在多孔陶瓷基体中,也可以是通过在多孔陶瓷基体上丝印导电层,同时需要将电极引线和多孔陶瓷基体烧结在一起,使得加热体与电极连接,而电极引线在烧结时的收缩率较大,如果多孔陶瓷的韧性不够,电极引线的收缩会将电极引线从陶瓷坯体结合处扯掉脱落,如何保证多孔陶瓷基体在满足韧性强度的要求下,同时具有与印刷导电层具有较高的结合强度,为本领域亟需解决的一个技术问题。
发明内容
针对上述问题,本公开提供了一种碱式多孔陶瓷基体及其制备方法、电子烟雾化芯和电子烟。
本公开解决上述技术问题所采用的技术方案如下:
一个方面,本公开提供了一种碱式多孔陶瓷基体,以所述碱式多孔陶瓷基体的总重量为基准,包括:
陶瓷粉体45~98.1份、氧化物助烧剂0.4~14份、碱金属氧化物1~15份、铌氧化物0.0005~0.25份和钇稳定的锆氧化物0.1~10份。
可选的,所述碱式多孔陶瓷基体中所述碱金属氧化物的含量为1.6~12份,所述铌氧化物的含量为0.01~0.15份,所述钇稳定的锆氧化物的含量为1~3份。
可选的,以所述碱式多孔陶瓷基体的总重量为基准,所述碱金属氧化物包括0.5~8份的氧化钠和0.5~7份的氧化钾。
可选的,所述铌氧化物包括五氧化二铌。
可选的,所述钇稳定的锆氧化物的比表面积为15-20m 2/g,中值粒径为0.1-0.15μm。
可选的,以所述碱式多孔陶瓷基体的总重量为基准,所述氧化物助烧剂包括以下重量组分:
镁氧化物0.2~7份和钙氧化物0.2~7份。
另一个方面,本公开提供了如上所述的碱式多孔陶瓷基体的制备方法,包括以下操作步骤:
将陶瓷粉体、氧化物助烧剂、碱金属氧化物、铌氧化物和钇稳定的锆氧化物按重量份数配比混合进行球磨,干燥得到复合粉体;
将复合粉体与造孔剂和粘结剂混合成型得到坯体;
将坯体进行烧结去除粘结剂和造孔剂得到碱式多孔陶瓷基体。
另一个方面,本公开提供一种碱式多孔陶瓷基体,由上述方法制备得到。
另一个方面,本公开提供了一种电子烟雾化芯,包括如上所述的碱式多孔陶瓷基体以及位于碱式多孔陶瓷基体表面的导电层。
另一个方面,本公开提供了一种电子烟,包括如上所述的电子烟雾化芯。
根据本公开提供的碱式多孔陶瓷基体,一方面保证了多孔陶瓷体的结构强度,防止了电极引线在烧结时出现收缩导致陶瓷基体脱落,另一方面使得陶瓷基体与印刷导电涂层的结合性能更强。
具体实施方式
为了使本公开所解决的技术问题、技术方案及有益效果更加清楚明白,以下结合实施例,对本公开进行进一步详细说明。应当理解,此处所描述的具体实施例仅仅用以解释本公开,并不用于限定本公开。
本公开实施例提供了一种碱式多孔陶瓷基体,以所述碱式多孔陶瓷基体的总重量为基准,包括:
陶瓷粉体45~98.1份、氧化物助烧剂0.4~14份、碱金属氧化物1~15份、铌氧化物0.0005~0.25份和钇稳定的锆氧化物0.1~10份。
本公开的发明人在实验过程中偶然发现,将碱金属氧化物、铌氧化物以及钇稳定的锆氧化物共同用于陶瓷雾化芯的陶瓷基体的制备中,制备得到的多孔陶瓷基体,一方面,不仅陶瓷基体的韧性强度得到了提高,另一方面,当通过丝网印刷的方式在陶瓷基体上印刷导电涂层通过烧结得到导电层时,陶瓷基体与导电层的结合强度具有一定的改善。
在优选的实施例中,所述碱金属氧化物的含量为1.6~12份,所述铌氧化物的含量为0.01~0.15份,所述钇稳定的锆氧化物的含量为1~3份。
根据本公开的实施例,所述钇稳定的锆氧化物为物相是四方相的氧化钇稳定氧化锆。
在一些实施例中,所述碱金属氧化物包括以下重量组分:
氧化钠0.5~8份和氧化钾0.5~7份。
在优选的实施例中,氧化钠和氧化钾的添加量为:氧化钠0.8~7份和氧化钾0.8~5份。
在一些实施例中,所述铌氧化物包括一氧化铌、二氧化铌、三氧化二铌和五氧化二铌中的一种或多种。
在优选的实施例中,所述铌氧化物选自于五氧化二铌。
五氧化二铌为铌的高价态氧化物,性质稳定,制备难度和成本相对于其他铌氧化物较低,可在空气中灼烧金属铌或由铌酸脱水制备。
在一些实施例中,所述钇稳定的锆氧化物的比表面积为15-20m 2/g,粒径中值为0.1-0.15μm。
在一些实施例中,所述钇稳定的锆氧化物中包括有2~4mol%的氧化钇。
所述钇稳定的锆氧化物在烧结的过程中形成四方晶相,所述氧化钇起到稳定其四方晶相的作用,提高力学性能,需要说明的是,单独加入氧化钇对防止电极引线脱落的效果提升改善有限,在本公开的技术方案中,所述钇稳定的锆氧化物仅在加入铌氧化物后才能达到防止电极引线脱落所要求的材料韧性。
所述陶瓷粉体在所述碱式多孔陶瓷基体中起到形成主体骨架的作用,在一些实施例中,所述陶瓷粉体包括铝氧化物、硅氧化物、硅藻土、长石、高岭土、蒙脱石、伊利石、堇青石、膨胀珍珠岩和黏土中的一种或多种。以上物质具有坚固、耐磨、耐高温、来源广泛,成本低廉的优点,作为陶瓷粉体时,确保了多孔陶瓷的强度和韧性。
在优选的实施例中,所述陶瓷粉体包括以下重量组分:
铝氧化物10~50份和硅氧化物35~85份。
在更优选的实施例中,铝氧化物和硅氧化物的添加量为:铝氧化物18~50份和硅氧化物40~77份。
采用铝氧化物和硅氧化物作为陶瓷粉体,相比于其他材料,其物质纯度具有较好的可控性,从而有利于提高产品质量的一致性。其中铝氧化物为高温陶瓷,起到骨架支撑的作用,硅氧化物在烧结的过程在晶界形成低熔点的玻璃相,促进烧结,对铝氧化物起到粘结的作用。
在一些实施例中,以所述碱式多孔陶瓷基体的总重量为基准,所述氧化物助烧剂包括以下重量组分:
镁氧化物0.2~7份和钙氧化物0.2~7份。
在优选的实施例中,镁氧化物和钙氧化物的添加量为:镁氧化物0.5~5份和钙氧化物0.5~5份。
在所述陶瓷粉体中加入所述镁氧化物,主要起到微观结构稳定剂的作用,可以细化晶粒,大大减小晶界能差,削弱晶粒生长的各向异性,抑制不连续的晶粒生长。
所述钙氧化物与所述镁氧化物相互配合,用于获得致密的显微组织和均匀细腻的晶粒。
本公开的另一实施例提供了如上所述的碱式多孔陶瓷基体的制备方法,包括以下操作步骤:
将陶瓷粉体、氧化物助烧剂、碱金属氧化物、铌氧化物和钇稳定的锆氧化物按重量份数配比混合进行球磨,干燥得到复合粉体;
将复合粉体与造孔剂和粘结剂混合成型得到坯体;
将坯体进行烧结去除粘结剂和造孔剂得到碱式多孔陶瓷基体。
具体的,以干压成型为例,所述碱式多孔陶瓷基体的制备方法包括以下操作步骤:
①先将陶瓷粉体、氧化物助烧剂、碱金属氧化物、铌氧化物和钇稳定的锆氧化物按照重量比例在球磨罐中加水球磨,然后再在砂磨机中加入分散剂和水砂磨,最后加入造孔剂和粘结剂搅拌,形成喷雾用浆料;
②将浆料送入喷雾塔进行喷雾干燥形成用来干压的流动性较强的球形粉体,之后将球形粉体干压成型(吨位200吨的压机使用8MPa的油压压强);
③在1000-1300度下烧结1-2小时,打磨抛光后即制成最终样品。
需要说明的是,以上干压成型仅是所述碱式多孔陶瓷基体的优选实施例,用于对本公开进行说明,并不用于对本公开进行限制,在其他实施例中,本领域技术人员可采用其他现有的成型方式进行所述碱式多孔陶瓷基体的制备,如等静压成型、注射成型、热压铸成型等成型方式。
本公开的另一实施例提供了如上述方法制备得到的碱式多孔陶瓷基体。
本公开的另一实施例提供了一种电子烟雾化芯,所述电子烟雾化芯包括碱式多孔陶瓷基体、导电层和电极引线,所述导电层位于所述碱式多孔陶瓷基体表面,所述电极引线插入所述碱式多孔陶瓷基体并电连接所述导电层;所述导电层通过将导电浆料丝印在碱式多孔陶瓷基体表面后经烧结得到。
在制备所述电子烟雾化芯时,所述导电层通过导电浆料丝印成型,所述电极引线插入所述碱式多孔陶瓷基体预设的雾化芯孔中后,在还原性气体炉中烧结固定,还原性气体选自氨气或氢气。
将所述碱式多孔陶瓷基体应用于电子烟雾化芯,在制备过程中,能够有效提高电极引线和所述碱式多孔陶瓷基体的结合强度,避免电极引线在烧结过程中脱落,同时又保证了丝印的效果,提高了导电层的结合力。
本公开的另一实施例提供了一种电子烟,包括如上所述的电子烟雾化芯。
以下通过实施例对本公开进行进一步的说明。
实施例1
提供一种碱式多孔陶瓷基体组合物,配料如下:
粉体:其中氧化铝加入25g,氧化硅加入66.48g,氧化镁加入1.5g,氧化钙加入3g,氧化钠加入1g,氧化钾加入1g,五氧化二铌加入0.02g,3mol%钇稳定的氧化锆加入2g。
造孔剂:PMMA(聚甲基丙烯酸甲酯)加入26g。
PVA粘结剂(聚乙烯醇)加入10g。
水分加入100g。
具体制备方法如下:
先将粉体在球磨罐里混料2小时,出料烘干后,进入烧结炉烧制1000℃保温1小时。烧成的粉破碎后,加入作为造孔剂的PMMA26g,PVA粘结剂10g以及水100g,搅拌混合 2小时,进行喷雾干燥,干燥后的粉体干压成型成电子烟雾化芯形状的坯体,之后进炉烧制1140℃保温1.5h。烧成的坯体丝印导电浆料并插入电极引线进入氢气炉烧制,烧制温度为1050℃,得到电子烟雾化芯。
实施例2
提供一种碱式多孔陶瓷基体组合物,配料如下:
粉体:其中氧化铝加入18g,氧化硅加入73.48g,氧化镁加入1.5g,氧化钙加入3g,氧化钠加入0.5g,氧化钾加入0.5g,五氧化二铌加入0.02g,3mol%钇稳定的氧化锆加入2g。
造孔剂:PMMA(聚甲基丙烯酸甲酯)加入26g。
PVA粘结剂(聚乙烯醇)加入10g。
水分加入100g。
具体制备方法如下:
先将粉体在球磨罐里混料2小时,出料烘干后,进入烧结炉烧制1000℃保温1小时。烧成的粉破碎后,加入作为造孔剂的PMMA26g,PVA粘结剂10g以及水100g,搅拌混合2小时,进行喷雾干燥,干燥后的粉体干压成型成电子烟雾化芯形状的坯体,之后进炉烧制1140℃保温1.5h。烧成的坯体丝印导电浆料并插入电极引线进入氢气炉烧制,烧制温度为1050℃,得到电子烟雾化芯。
实施例3
提供一种碱式多孔陶瓷基体组合物,配料如下:
粉体:其中氧化铝加入50g,氧化硅加入41.48g,氧化镁加入1.5g,氧化钙加入3g,氧化钠加入2g,氧化钾加入2g,五氧化二铌加入0.02g,3mol%钇稳定的氧化锆加入2g。
造孔剂:PMMA(聚甲基丙烯酸甲酯)加入26g。
PVA粘结剂(聚乙烯醇)加入10g。
水分加入100g。
具体制备方法如下:
先将粉体在球磨罐里混料2小时,出料烘干后,进入烧结炉烧制1000℃保温1小时。烧成的粉破碎后,加入作为造孔剂的PMMA26g,PVA粘结剂10g以及水100g,搅拌混合2小时,进行喷雾干燥,干燥后的粉体干压成型成电子烟雾化芯形状的坯体,之后进炉烧 制1235℃保温1.5h。烧成的坯体丝印导电浆料并插入电极引线进入氢气炉烧制,烧制温度为1050℃,得到电子烟雾化芯。
实施例4
提供一种碱式多孔陶瓷基体组合物,配料如下:
粉体:其中氧化铝加入25g,氧化硅加入67.49g,氧化镁加入1.5g,氧化钙加入3g,氧化钠加入5g,氧化钾加入5g,五氧化二铌加入0.01g,3mol%钇稳定的氧化锆加入1g。
造孔剂:PMMA(聚甲基丙烯酸甲酯)加入26g。
PVA粘结剂(聚乙烯醇)加入10g。
水分加入100g。
具体制备方法如下:
先将粉体在球磨罐里混料2小时,出料烘干后,进入烧结炉烧制1000℃保温1小时。烧成的粉破碎后,加入作为造孔剂的PMMA26g,PVA粘结剂10g以及水100g,搅拌混合2小时,进行喷雾干燥,干燥后的粉体干压成型成电子烟雾化芯形状的坯体,之后进炉烧制1170℃保温1.5h。烧成的坯体丝印导电浆料并插入电极引线进入氢气炉烧制,烧制温度为1050℃,得到电子烟雾化芯。
实施例5
提供一种碱式多孔陶瓷基体组合物,配料如下:
粉体:其中氧化铝加入25g,氧化硅加入65.35g,氧化镁加入1.5g,氧化钙加入3g,氧化钠加入7g,氧化钾加入8g,五氧化二铌加入0.15g,3mol%钇稳定的氧化锆加入3g。
造孔剂:PMMA(聚甲基丙烯酸甲酯)加入26g。
PVA粘结剂(聚乙烯醇)加入10g。
水分加入100g。
具体制备方法如下:
先将粉体在球磨罐里混料2小时,出料烘干后,进入烧结炉烧制1000℃保温1小时。烧成的粉破碎后,加入作为造孔剂的PMMA26g,PVA粘结剂10g以及水100g,搅拌混合2小时,进行喷雾干燥,干燥后的粉体干压成型成电子烟雾化芯形状的坯体,之后进炉烧制1100℃保温1.5h。烧成的坯体丝印导电浆料并插入电极引线进入氢气炉烧制,烧制温度 为1050℃,得到电子烟雾化芯。
对比例1
提供一种多孔陶瓷基体组合物,配料如下:
粉体:其中氧化铝加入25g,氧化硅加入66.48g,氧化镁加入1.5g,氧化钙加入3g,氧化铋加入2g,五氧化二铌加入0.02g,3mol%钇稳定的氧化锆加入2g。
造孔剂:PMMA(聚甲基丙烯酸甲酯)加入26g。
PVA粘结剂(聚乙烯醇)加入10g。
水分加入100g。
具体制备方法如下:
先将粉体在球磨罐里混料2小时,出料烘干后,进入烧结炉烧制1000℃保温1小时。烧成的粉破碎后,加入作为造孔剂的PMMA26g,PVA粘结剂10g以及水100g,搅拌混合2小时,进行喷雾干燥,干燥后的粉体干压成型成电子烟雾化芯形状的坯体,之后进炉烧制1070℃保温1.5h。烧成的坯体丝印导电浆料并插入电极引线进入氢气炉烧制,烧制温度为1050℃,得到电子烟雾化芯。
对比例2
提供一种多孔陶瓷基体组合物,配料如下:
粉体:其中氧化铝加入25g,氧化硅加入66.48g,氧化镁加入1.5g,氧化钙加入3g,氧化钠加入1g,氧化钾加入1g,3mol%钇稳定的氧化锆加入2g。
造孔剂:PMMA(聚甲基丙烯酸甲酯)加入26g。
PVA粘结剂(聚乙烯醇)加入10g。
水分加入100g。
具体制备方法如下:
先将粉体在球磨罐里混料2小时,出料烘干后,进入烧结炉烧制1000℃保温1小时。烧成的粉破碎后,加入作为造孔剂的PMMA26g,PVA粘结剂10g以及水100g,搅拌混合2小时,进行喷雾干燥,干燥后的粉体干压成型成电子烟雾化芯形状的坯体,之后进炉烧制1140℃保温1.5h。烧成的坯体丝印导电浆料并插入电极引线进入氢气炉烧制,烧制温度为1050℃,得到电子烟雾化芯。
对比例3
提供一种多孔陶瓷基体组合物,配料如下:
粉体:其中氧化铝加入25g,氧化硅加入66.48g,氧化镁加入1.5g,氧化钙加入3g,氧化钠加入1g,氧化钾加入1g,五氧化二铌加入0.02g。
造孔剂:PMMA(聚甲基丙烯酸甲酯)加入26g。
PVA粘结剂(聚乙烯醇)加入10g。
水分加入100g。
具体制备方法如下:
先将粉体在球磨罐里混料2小时,出料烘干后,进入烧结炉烧制1000℃保温1小时。烧成的粉破碎后,加入作为造孔剂的PMMA26g,PVA粘结剂10g以及水100g,搅拌混合2小时,进行喷雾干燥,干燥后的粉体干压成型成电子烟雾化芯形状的坯体,之后进炉烧制1170℃保温1.5h。烧成的坯体丝印导电浆料并插入电极引线进入氢气炉烧制,烧制温度为1050℃,得到电子烟雾化芯。
性能测试
对上述实施例1~5和对比例1~3制备得到的电子烟雾化芯进行如下性能测试:
导热率测试:依照标准ASTM518的方式,使用热导率仪测试电子烟雾化芯的导热率。
强度测试:依照标准GB/T 6569-86的方式,使用万能试验机进行电子烟雾化芯的强度测试。
拉拔力测试:固定电子烟雾化芯,通过拉力计固定电极引线,将电极引线从电子烟雾化芯中扯下,记录所用的拉拔力。
陶瓷基体与导电层的结合强度测试:将电子烟雾化芯置于60度下加热两秒,再置于10度在冷却5秒,作为一次冷热冲击测试,当导电层出现脱落时,记录电子烟雾化芯的冷热冲击测试次数。
得到的测试结果填入表1。
表1
具体事例 强度(MPa) 拉拔力(N) 导热率(W/(mK)) 冷热冲击次数
实施例1 52 11 1.3 12
实施例2 47 9 1.1 7
实施例3 49 10 1.5 10
实施例4 45 8 1.2 6
实施例5 50 10 1.4 11
对比例1 49 9 1.2 5
对比例2 36 4 1.3 11
对比例3 30 4 1.1 10
对比实施例1~5和对比例1的测试结果可以看出,相比于不添加碱金属氧化物的多孔陶瓷基体,采用本公开提供的添加碱金属氧化物、铌氧化物以及钇稳定的锆氧化物共同添加得到的碱式多孔陶瓷基体,其耐冷热冲击的次数更高,说明碱金属氧化物、铌氧化物以及钇稳定的锆氧化物的配合有利于改善碱式多孔陶瓷基体与导电层的结合强度。
对比实施例1~5和对比例2、3的测试结果可以看出,碱金属氧化物、铌氧化物以及钇稳定的锆氧化物共同添加能够有效提高碱式多孔陶瓷基体的材料强度和韧性,进而使得碱式多孔陶瓷基体与电极引线之间的结合强度有效提高,避免电极引线的脱落,当缺少其中的铌氧化物或钇稳定的锆氧化物时均会导致碱式多孔陶瓷基体的强度下降,进而引起电极引线的脱落。
以上所述仅为本公开的较佳实施例而已,并不用以限制本公开,凡在本公开的精神和原则之内所作的任何修改、等同替换和改进等,均应包含在本公开的保护范围之内。

Claims (10)

  1. 一种碱式多孔陶瓷基体,其特征在于,以所述碱式多孔陶瓷基体的总重量为基准,包括:
    陶瓷粉体45~98.1份、氧化物助烧剂0.4~14份、碱金属氧化物1~15份、铌氧化物0.0005~0.25份和钇稳定的锆氧化物0.1~10份。
  2. 根据权利要求1所述的碱式多孔陶瓷基体,其特征在于,所述碱式多孔陶瓷基体中碱金属氧化物的含量为1.6~12份,所述铌氧化物的含量为0.01~0.15份,所述钇稳定的锆氧化物的含量为1~3份。
  3. 根据权利要求1或2所述的碱式多孔陶瓷基体,其特征在于,以所述碱式多孔陶瓷基体的总重量为基准,所述碱金属氧化物包括0.5~8份的氧化钠和0.5~7份的氧化钾。
  4. 根据权利要求1至3中任一项所述的碱式多孔陶瓷基体,其特征在于,所述铌氧化物包括五氧化二铌。
  5. 根据权利要求1至4中任一项所述的碱式多孔陶瓷基体,其特征在于,所述钇稳定的锆氧化物的比表面积为15-20m 2/g,中值粒径为0.1-0.15μm。
  6. 根据权利要求1至5中任一项所述的碱式多孔陶瓷基体,其特征在于,以所述碱式多孔陶瓷基体的总重量为基准,所述氧化物助烧剂包括以下重量组分:
    镁氧化物0.2~7份和钙氧化物0.2~7份。
  7. 如权利要求1至6中任一项所述的碱式多孔陶瓷基体的制备方法,其特征在于,包括以下操作步骤:
    将陶瓷粉体、氧化物助烧剂、碱金属氧化物、铌氧化物和钇稳定的锆氧化物按重量份数配比混合进行球磨,干燥得到复合粉体;
    将复合粉体与造孔剂和粘结剂混合成型得到坯体;
    将坯体进行烧结去除粘结剂和造孔剂得到碱式多孔陶瓷基体。
  8. 一种碱式多孔陶瓷基体,由权利要求7所述的方法制备得到。
  9. 一种电子烟雾化芯,其特征在于,包括权利要求1至6以及8中任意一项所述的碱式多孔陶瓷基体以及位于碱式多孔陶瓷基体表面的导电层。
  10. 一种电子烟,其特征在于,包括权利要求9所述的电子烟雾化芯。
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