CN113292354A - 多孔陶瓷雾化芯及其制备方法 - Google Patents

多孔陶瓷雾化芯及其制备方法 Download PDF

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CN113292354A
CN113292354A CN202110649959.8A CN202110649959A CN113292354A CN 113292354 A CN113292354 A CN 113292354A CN 202110649959 A CN202110649959 A CN 202110649959A CN 113292354 A CN113292354 A CN 113292354A
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porous ceramic
atomizing core
preparing
ceramic atomizing
coupling agent
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余明先
张霖
王伟江
刘友昌
戴高环
王超
何培与
何晓刚
姚伟昌
李毅
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Shenzhen Taotao Technology Co ltd
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Abstract

本发明提供一种多孔陶瓷雾化芯的制备方法，包括以下步骤：提供制备雾化芯的多孔陶瓷；将所述多孔陶瓷浸泡于溶液中，取出浸泡后的多孔陶瓷，并将其置于水蒸汽中进行原位水解反应，将原位水解反应后的多孔陶瓷进行烧结，得到表面覆盖有纳米粒子层的多孔陶瓷雾化芯；其中，所述溶液为将第一物质溶于有机溶剂中制得，所述第一物质包括有机硅、三甲基铝或二乙基锌中的至少一种；所述纳米粒子层包括SiO2、A l 2O3或ZnO中的至少一种。还提供一种由上述制备方法制备而成的多孔陶瓷雾化芯。本发明提供的多孔陶瓷雾化芯结构简单，其制备方法也非常简单，且无需另外增加气动结构即可实现烟油的有效渗透，增大了电子烟的雾化量，使用户体验感更好。

Description

多孔陶瓷雾化芯及其制备方法
技术领域
本发明属于多孔陶瓷技术领域，特别是涉及多孔陶瓷雾化芯及其制备方法。
背景技术
现有多孔陶瓷雾化芯，其储油槽内的烟油在压差的作用下通过陶瓷孔浸渗至雾化面上，其压差的形成需要在雾化芯上设置连通外界环境的气动结构，且压差须维持稳定以保证烟油持续稳定浸渗，此种结构一方面增加了雾化芯的制备难度，另一方面，由于抽吸电子烟时，气流很难保持稳定，储油槽上的压差难免会有比较大的波动，这样就使得烟油无法稳定地浸渗到雾化面上，无法及时给雾化面提供足够的烟油，导致电子烟的雾化量小，用户体验差。
发明内容
本发明的目的在于克服现有技术中存在的不足，并提供一种多孔陶瓷雾化芯及其制备方法，该制备方法简单，制备的多孔陶瓷雾化芯结构简单，且无需另外增加气动结构即可实现烟油的有效渗透，增大了电子烟的雾化量，使用户体验感更好。
为实现上述目的，本发明采用的技术方案为：
一种多孔陶瓷雾化芯的制备方法，包括以下步骤：
提供制备雾化芯的多孔陶瓷；
将所述多孔陶瓷浸泡于溶液中，取出浸泡后的多孔陶瓷，并将其置于水蒸汽中进行原位水解反应，将原位水解反应后的多孔陶瓷进行烧结，得到表面覆盖有纳米粒子层的多孔陶瓷雾化芯；其中，所述溶液为将第一物质溶于有机溶剂中制得，所述第一物质包括有机硅、三甲基铝或二乙基锌中的至少一种；所述纳米粒子层包括SiO2、Al2O3或ZnO中的至少一种。
对上述技术方案的进一步改进是：
所述纳米粒子层的粒径范围为50～150nm。
制备所述多孔陶瓷的原料为硅藻土、云母或麦饭石。
所述烧结时的温度范围为1000～1200℃。
在将原位水解反应后的多孔陶瓷进行烧结后，还包括以下步骤：
配制偶联剂与乙醇的混合液，所述混合液中偶联剂与乙醇的体积比为2～5：100，所述偶联剂为硅烷偶联剂；将表面覆盖有纳米粒子层的多孔陶瓷雾化芯浸泡到所述混合液中，取出后进行干燥处理，得到吸附有偶联剂的多孔陶瓷雾化芯。
所述偶联剂包括γ-氨丙基三乙氧基硅烷、γ-(2，3-环氧丙氧)丙基三甲氧基硅烷、γ-(甲基丙烯酰氧)丙基三甲氧基硅烷、，N-β-(氨乙基)-γ-氨丙基三甲氧基硅烷、乙烯基三(β-甲氧基乙氧基)硅烷中的至少一种。
所述浸泡的时间为12～24h。
所述干燥处理的温度范围为80～110℃。
在进行干燥处理后，还包括以下步骤：
在吸附有偶联剂的多孔陶瓷雾化芯表面包覆纳米膜层，所述纳米膜层包括SiO2、Al2O3或ZnO中的至少一种。
本发明还提供一种多孔陶瓷雾化芯，由上述的制备方法制备而成。
根据本发明的技术方案可知，本发明的多孔陶瓷雾化芯的制备方法，其首先提供了制备雾化芯的多孔陶瓷，再将多孔陶瓷浸泡于溶液中，使无机物前驱体源吸附在多孔陶瓷上，将多孔陶瓷取出后，在水蒸汽的作用下，陶瓷孔洞相当于微型反应器，无机物前驱体源和水蒸汽在陶瓷孔洞内发生原位水解反应，再通过后面的高温烧结后，能够在多孔陶瓷上形成分布均匀的无机氧化物纳米粒子层。该纳米粒子层具有良好的亲油效果，使多孔陶瓷的陶瓷孔超亲油，烟油更容易润湿陶瓷孔的壁面，从而实现在不需要压差的条件下，即可使烟油顺利通过陶瓷孔，浸渗到雾化面上，及时给雾化面提供充足的烟油，增大电子烟的雾化量，使用户体验感更好。
附图说明
图1为本发明实施例3多孔陶瓷雾化芯的制备方法的流程示意图。
具体实施方式
为了便于理解本发明，下面将参照相关附图对本发明进行更全面的描述。附图中给出了本发明的较佳实施例。但是，本发明可以以许多不同的形式来实现，并不限于本文所描述的实施例。相反地，提供这些实施例的目的是使对本发明的公开内容的理解更加透彻全面。
除非另有定义，本文所使用的所有的技术和科学术语与属于本发明的技术领域的技术人员通常理解的含义相同。本文中在本发明的说明书中所使用的术语只是为了描述具体的实施例的目的，不是旨在于限制本发明。
如图1所示，本实施例的多孔陶瓷雾化芯的制备方法，包括以下步骤：
S1、提供多孔陶瓷：提供制备雾化芯的多孔陶瓷，所述多孔陶瓷的制备方法如下：
S1.1、陶瓷粉体表面改性：将陶瓷粉体与表面改性剂混合后，共同进行球磨预处理，得到表面改性陶瓷粉体。
本实施例中具体为，以天然微孔硅藻土、云母或麦饭石为陶瓷粉体，所述陶瓷粉体的粒径为15μm。将所述陶瓷粉体与表面改性剂混合后，共同进行球磨预处理，使陶瓷粉体表面形成一层包覆层，烘干后得到表面改性陶瓷粉体。所述陶瓷粉体与表面改性剂的质量比为100：1，所述包覆层的厚度为10nm。
所述表面改性剂由硬脂酸、油酸、十二羟基硬脂酸和柠檬酸中的至少一种组成，且每100质量份的所述陶瓷粉体中，加入的表面改性剂的质量份数为1～5份。
陶瓷粉体的粒径小，且颗粒均匀，更有利于与表面改性剂混合均匀，从而使其结合性更好，有利于提高陶瓷的强度。
S1.2、混合喂料制备：将有机胶体系与步骤S1制得的表面改性陶瓷粉体混合后得到混合喂料。
具体为，首先对有机胶体系进行密炼，再将密炼后的有机胶体系与步骤S1制得的表面改性陶瓷粉体混合后得到混合喂料,其中，混合喂料与有机胶体系的质量比为100：15。
所述有机胶体系包括硅橡胶胶粘剂(PW)、硬脂酸(SA)、聚乙烯(PE)、聚丙烯(PP)和树脂；其质量配比PW:SA:PE:PP:树脂＝37:3:25:20:15。
有机胶体系密炼步骤:先将PW放入W型对辊密炼机中加热，待PW呈熔融状态，且液态PW的温度达到200℃后，分别加入树脂、PE和PP，启动密炼机，密炼30min后加入SA，再继续密炼4h后结束密炼，密炼时加微正压100Pa。
S1.3、注射成型：将步骤S2制得的混合喂料放入到螺杆式注射机中，进行注射成型，得到多孔陶瓷生坯。注射成型时的成型温度为120℃，成型压力为120MPa。
S1.4、脱脂步骤：使用溶剂将步骤S3中制得的多孔陶瓷生坯中的表面改性剂和有机胶体系脱出，得到溶剂脱脂生坯。
具体为，以煤油、汽油或白电油中的一种作为有机溶剂，在恒温油浴锅中，将步骤S3制得的陶瓷雾化芯生坯完全浸泡在有机溶剂中，并加热至120℃，保温20h。通过有机溶剂萃取脱脂，将陶瓷雾化芯生坯中的表面改性剂和有机胶体系中可溶于有机溶剂的组分去除，得到溶剂脱脂生坯。
将溶剂脱脂生坯置于水浴锅中进一步脱脂和清洗，水浴温度为80℃，时间为24h，得到水浴脱脂生坯。水浴萃取脱脂可以进一步去除陶瓷雾化芯生坯中的水溶性有机组分。
将水浴脱脂生坯置于马弗炉中干燥12h，干燥温度为90℃，加热时升温速度为4℃/min，最终得到脱脂生坯。
S1.5、烧结步骤：将步骤S4制得的脱脂生坯置于恒温加压设备中，施加高压低温，采用热压法进行烧结。所述低温的温度为200℃，所述高压的压力为350MPa，保温保压时间为30min，得到多孔陶瓷。
本实施例中，有机胶体系作为造孔剂，依靠酚醛树脂提供结合强度，使多孔陶瓷生坯在脱脂之后形成具有一定强度的多孔结构陶瓷，多孔结构有利于提高雾化芯的吸油速率，而强度的提高则有助于提高雾化芯的使用寿命。
上述方法仅为多孔陶瓷雾化芯制备的一个具体实施例，实际应用中，并不限制多孔陶瓷的具体制备方法。
S2、制备纳米粒子层：将所述多孔陶瓷浸泡于溶液中，浸泡时间为1～10h；取出浸泡后的多孔陶瓷，并将其置于水蒸汽中进行原位水解反应，水解反应的时间为1～10h；将原位水解反应后的多孔陶瓷进行烧结，烧结温度为1000～1200℃，烧结时间为1～5h，得到表面覆盖有纳米粒子层的多孔陶瓷雾化芯。其中，所述溶液为将第一物质溶于有机溶剂中制得，所述第一物质包括有机硅、三甲基铝或二乙基锌中的至少一种；所述纳米粒子层包括SiO2、Al2O3或ZnO中的至少一种。
所述纳米粒子层的粒径范围为50～150nm，可以通过控制有机硅、三甲基铝或二乙基锌在溶液中的浓度和水解反应时长来控制粒径的范围。所述有机溶剂为醇溶剂，比如可以是乙醇、丁醇、丙二醇醚类等。
在步骤S2中，无机物前驱体源(SiO2、Al2O3或ZnO)能够在水蒸汽的作用下，发生原位水解反应，并在后续的高温烧结后在多孔陶瓷上形成无机氧化物纳米粒子层。纳米粒子层的形成，可以使雾化芯具有更好的亲油效果，使烟油更易浸渗。
本实施例制备的多孔陶瓷，通过视频光学接触角测量仪检测，其表面的烟油油滴的接触角α介于20°和30°之间，即20°≤α≤30°
实施例2：本实施例的多孔陶瓷雾化芯的制备方法，为使多孔陶瓷雾化芯具有更好的亲油效果，除包括实施例1的具体步骤外，还可以包括以下步骤：
S3、包覆偶联剂：配制偶联剂与乙醇的混合液，并进行充分搅拌，使其混合均匀，所述混合液中偶联剂与乙醇的体积比为2～5：100，所述偶联剂为硅烷偶联剂；将表面覆盖有纳米粒子层的多孔陶瓷雾化芯浸泡到所述混合液中，浸泡时间为12～24h；取出后洗净，进行干燥处理，干燥处理的温度范围为80～110℃，干燥处理时间为0.5～5h，得到吸附有偶联剂的多孔陶瓷雾化芯。
所述偶联剂包括γ-氨丙基三乙氧基硅烷、γ-(2，3-环氧丙氧)丙基三甲氧基硅烷、γ-(甲基丙烯酰氧)丙基三甲氧基硅烷、，N-β-(氨乙基)-γ-氨丙基三甲氧基硅烷、乙烯基三(β-甲氧基乙氧基)硅烷中的至少一种。
本实施例中所使用的偶联剂由两部分组成，包括亲无机基团和亲有机基团，新无机基团能够和硅藻土牢固结合，而亲有机基团则暴露于多孔陶瓷的表面，具有良好的亲油效果。
本实施例制备的多孔陶瓷，经检测其表面的烟油油滴的接触角α介于5°和20°之间，即5°≤α＜20°。
实施例3：本实施例的多孔陶瓷雾化芯的制备方法，为使吸附的偶联剂与多孔陶瓷结合的更为紧密，除实施例2的具体步骤外，还可包括以下步骤：
S4、制备纳米膜层：在吸附有偶联剂的多孔陶瓷雾化芯表面采用低温沉积法(ALD)包覆纳米膜层，所述纳米膜层包括SiO2、Al2O3或ZnO中的至少一种。
纳米膜层的制备，能够稳定吸附的偶联剂，降低其在多孔陶瓷表面的脱附的可能性，同时还可以提高雾化芯的亲油性，使烟油更易于渗透。
本发明多孔陶瓷雾化芯的制备方法中最优的实施例中，多孔陶瓷的表面覆盖了三层结构，从内到外，依次为纳米粒子层、偶联剂层和纳米膜层，三层结构不仅使其与多孔陶瓷的结合更为紧密，而且使雾化芯具有更好的亲油效果，使烟油更易于渗透到雾化面上，使电子烟的雾化量更大。
本实施例制备的多孔陶瓷，经检测其表面的烟油油滴的接触角α小于5°，即α＜5°
经检测，本发明三个实施例中，实施例1中的烟油油滴的接触角最大时也未超过30°，而实施例3中的烟油油滴的接触角更小，不到5°，而测得的多孔陶瓷本身的表面的烟油油滴的接触角α介于60°和100°之间，即60°≤α≤100°，由检测结果可知，本发明方法制备的多孔陶瓷雾化芯具有更小的表面的烟油油滴的接触角，表明由本发明方法制备的多孔陶瓷雾化芯表面更加亲油，烟油油滴更易润湿雾化芯，烟油油滴能够在不需要压差的条件下，顺利通过雾化芯，到达雾化面，为雾化面提供足够的烟油，增大抽吸时的烟雾量，使用户体验感更好。
以上实施例的各技术特征可以进行任意的组合，为使描述简洁，未对上述实施例中的各个技术特征所有可能的组合都进行描述，然而，只要这些技术特征的组合不存在矛盾，都应当认为是本说明书记载的范围。
以上实施例仅表达了本发明的优选的实施方式，其描述较为具体和详细，但并不能因此而理解为对发明专利范围的限制。应当指出的是，对于本领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干变形和改进，这些都属于本发明的保护范围。因此，本发明专利的保护范围应以所附权利要求为准。

Claims (10)

1.一种多孔陶瓷雾化芯的制备方法，其特征在于：包括以下步骤：
提供制备雾化芯的多孔陶瓷；
将所述多孔陶瓷浸泡于溶液中，取出浸泡后的多孔陶瓷，并将其置于水蒸汽中进行原位水解反应，将原位水解反应后的多孔陶瓷进行烧结，得到表面覆盖有纳米粒子层的多孔陶瓷雾化芯；其中，所述溶液为将第一物质溶于有机溶剂中制得，所述第一物质包括有机硅、三甲基铝或二乙基锌中的至少一种；所述纳米粒子层包括SiO2、Al2O3或ZnO中的至少一种。
2.根据权利要求1所述的多孔陶瓷雾化芯的制备方法，其特征在于：所述纳米粒子层的粒径范围为50～150nm。
3.根据权利要求1所述的多孔陶瓷雾化芯的制备方法，其特征在于：制备所述多孔陶瓷的原料为硅藻土、云母或麦饭石。
4.根据权利要求1所述的多孔陶瓷雾化芯的制备方法，其特征在于：所述烧结时的温度范围为1000～1200℃。
5.根据权利要求1所述的多孔陶瓷雾化芯的制备方法，其特征在于：在将原位水解反应后的多孔陶瓷进行烧结后，还包括以下步骤：
配制偶联剂与乙醇的混合液，所述混合液中偶联剂与乙醇的体积比为2～5：100，所述偶联剂为硅烷偶联剂；将表面覆盖有纳米粒子层的多孔陶瓷雾化芯浸泡到所述混合液中，取出后进行干燥处理，得到吸附有偶联剂的多孔陶瓷雾化芯。
6.根据权利要求5所述的多孔陶瓷雾化芯的制备方法，其特征在于：所述偶联剂包括γ-氨丙基三乙氧基硅烷、γ-(2，3-环氧丙氧)丙基三甲氧基硅烷、γ-(甲基丙烯酰氧)丙基三甲氧基硅烷、，N-β-(氨乙基)-γ-氨丙基三甲氧基硅烷、乙烯基三(β-甲氧基乙氧基)硅烷中的至少一种。
7.根据权利要求5所述的多孔陶瓷雾化芯的制备方法，其特征在于：所述浸泡的时间为12～24h。
8.根据权利要求5所述的多孔陶瓷雾化芯的制备方法，其特征在于：所述干燥处理的温度范围为80～110℃。
9.根据权利要求5所述的多孔陶瓷雾化芯的制备方法，其特征在于：在进行干燥处理后，还包括以下步骤：
在吸附有偶联剂的多孔陶瓷雾化芯表面包覆纳米膜层，所述纳米膜层包括SiO2、Al2O3或ZnO中的至少一种。
10.一种多孔陶瓷雾化芯，其特征在于：由权利要求1至9任意一项所述的制备方法制备而成。
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