CN112592200B - 雾化芯用纳米多孔陶瓷及其制备方法 - Google Patents

雾化芯用纳米多孔陶瓷及其制备方法 Download PDF

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CN112592200B
CN112592200B CN202011561865.7A CN202011561865A CN112592200B CN 112592200 B CN112592200 B CN 112592200B CN 202011561865 A CN202011561865 A CN 202011561865A CN 112592200 B CN112592200 B CN 112592200B
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nano
ceramic
parts
paraffin
atomizing core
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CN112592200A (zh
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林光榕
秦飞
刘卫丽
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Huizhou Happy Vaping Technology Ltd
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Huizhou Happy Vaping Technology Ltd
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Priority to JP2023535581A priority Critical patent/JP2023553454A/ja
Priority to PCT/CN2021/128933 priority patent/WO2022127429A1/zh
Priority to EP21905358.4A priority patent/EP4245740A1/en
Priority to US18/211,287 priority patent/US20230331632A1/en
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Abstract

本发明雾化芯用纳米多孔陶瓷及制备方法，所述陶瓷包括：纳米氧化硅1～60份，陶瓷粉体10～80份，造孔剂1～50份，烧结助剂1～40份。制备方法包括：⑴称取纳米二氧化硅、陶瓷粉体、造孔剂、烧结助剂原料，置于球磨装置中混合球磨；⑵将球磨后的混合料烘烤干燥，得到混合粉料；⑶将石蜡加热至融化状态，边搅拌边加入混合粉料，加入完毕后继续搅拌1～8h，得到石蜡浆料；⑷将石蜡浆料注入预先准备的模具中，冷却成型，脱模得到蜡模；⑸将蜡模预加热进行除蜡，得到除蜡样；⑹将除蜡样进行烧结、降温，得到纳米多孔陶瓷。其有益效果是，解决了现有技术不能同时满足高孔隙率和高强度要求的问题，以及解决了杂质和重金属容易析出的问题。

Description

雾化芯用纳米多孔陶瓷及其制备方法
技术领域
本发明属于雾化芯技术领域，特别涉及一种雾化芯用纳米多孔陶瓷及其制备方法。
背景技术
雾化芯主要用于电子雾化器中，将待雾化液体进行加热雾化成气溶胶或蒸汽、汽雾，以便用户吸食。待雾化的液体可以是烟液或含有药物的溶液，用于健康医疗之用途。
目前雾化芯包括了多孔陶瓷为基材制成作为发热体，多孔陶瓷发热体主要是采用多孔陶瓷基体烧结的工艺，并在较低的温度下烧结。现有多孔陶瓷雾化芯及其制备方法是采用常规陶瓷粉体经过研磨后混合作为陶瓷粉体材料，降低烧结温度的方法是通过添加玻璃粉或石英砂实现，其软化温度点低，但制得的产品抗冷热冲击能力差，陶瓷在反复使用中会产生开裂漏油的问题，在结构不稳定的情况下，陶瓷内部的杂质和重金属容易分离出来混入待雾化的液体中，给人体带来潜在的危害。同时由于烧结温度低，为了保证产品的结构强度，通常采用降低孔隙率的方法解决，而产品孔隙率低，会导致产品在使用过程中容易积碳产生异味。
发明内容
本发明所解决的技术问题是克服现有技术不能同时满足高孔隙率和高强度要求的不足，以及解决强度结构不稳定的情况下，陶瓷内部的杂质和重金属容易分离出来混入待雾化的液体中，给人体带来潜在危害的问题，而提供一种雾化芯用纳米多孔陶瓷及其制备方法。
本发明的技术解决方案是所述雾化芯用纳米多孔陶瓷，其特殊之处在于，按重量份包括以下组分：纳米氧化硅1～60份，陶瓷粉体10～80份，造孔剂1～50份，烧结助剂1～40份。
优选地，按重量份包括以下组分：纳米氧化硅5～40份，陶瓷粉体20～70份，造孔剂5～30份，烧结助剂1～20份。
优选地，所述纳米氧化硅包括胶体的纳米二氧化硅或粉体的纳米二氧化硅，其纳米颗粒的一次粒径为10～150nm，胶体的纳米二氧化硅的量以其中固体份二氧化硅计。
优选地，所述陶瓷粉体包括高岭土、硅藻土、氧化铝、氮化硅、碳化硅、石英砂、玻璃砂、黏土、长石粉中的至少一种。
优选地，所述造孔剂包括石墨、淀粉、面粉、豆粉、聚苯乙烯微球、聚甲基丙烯酸甲酯微球、碳酸盐、铵盐、蔗糖、纤维中的至少一种，所述造孔剂粒径为1～200微米。
优选地，所述造孔剂为粒径1～20微米的鳞片状石墨。
优选地，所述烧结助剂包括氧化硼、硼酸、油酸、硬脂酸、硅酸钠、氧化钙、氧化铁、氧化钛中的至少一种。
本发明的另一种技术解决方案是，所述雾化芯用纳米多孔陶瓷的制备方法，包括以下步骤：
⑴按照配方称取纳米二氧化硅、陶瓷粉体、造孔剂、烧结助剂原料，置于球磨装置中混合球磨；
⑵将步骤⑴球磨后的混合料烘烤干燥，得到球磨干燥后的混合粉料；
⑶将石蜡加热至融化状态，边搅拌边加入所述混合粉料，加入完毕后继续搅拌1～8h，得到石蜡浆料；
⑷将所述石蜡浆料注入预先准备的模具中，冷却成型，脱模得到蜡模；
⑸将所述蜡模预加热进行除蜡，得到除蜡样；
⑹将所述除蜡样进行烧结，烧结过程包括升温、保温、降温，得到纳米多孔陶瓷。
优选地，步骤⑴所述球磨机转速为150～500rpm，球磨时间为1～10h，磨料直径为1～50mm。
优选地，步骤⑵所述烘烤干燥温度为60～150℃，干燥时间为至少1h，所述石蜡熔点为50～120℃，石蜡的添加量为混合粉料重量的10～60％。
优选地，步骤⑸所述除蜡温度为400～800℃，除蜡时间为2～12h。
优选地，步骤⑹所述烧结温度为600～1500℃，升温速度1～10℃/min，保温时间为2～12h。
优选地，步骤⑹所述烧结过程在保护气氛下进行，所述保护气氛为还原性氢气气氛、惰性气氛中的一种或多种。
与现有技术相比，本发明的有益效果：
多孔陶瓷制备过程中引入设定比例的纳米氧化硅材料，纳米级氧化硅与微米级的陶瓷粉体基料按设定比例进行混配，在煅烧过程中通过固化反应形成微纳米复合结构，纳米氧化硅由于其超高比表面积，且表面含有大量的羟基，在与陶瓷粉体固相反应时能有效降低烧结温度，同时该材料在高孔隙率的条件下可以使产品保持高强度，纳米氧化硅表面的多羟基结构促进陶瓷粉体间的固相反应，提高铝硅酸盐的转换效率，通过形成微纳结构提高了多孔陶瓷骨架结构的稳定性，因而具有高强度、低烧结温度、保持高孔隙率的特点，同时还可通过调节造孔剂的添加量在30～65％范围内调节孔隙率，制成的产品耐热冲击性好，性能稳定，在高强度、内部结构稳定的条件下，使得纳米多孔陶瓷不易碎裂，解决了陶瓷在反复使用中会产生开裂漏油的问题，且其结构的稳定性使产品在使用过程中不易分离出杂质和析出重金属，解决了杂质或重金属超标的问题，其高孔隙率解决了产品在使用过程中容易积碳产生异味的问题。
具体实施方式
本发明下面将结合实施例作进一步详述：
本发明的一种雾化芯用纳米多孔陶瓷，按重量份包括以下组分：纳米氧化硅1～60份，陶瓷粉体10～80份，造孔剂1～50份，烧结助剂1～40份。另外，为获得较佳效果，也可以按重量份包括以下组分：纳米氧化硅5～40份，陶瓷粉体20～70份，造孔剂5～30份，烧结助剂1～20份。
其中，纳米氧化硅包括胶体的纳米二氧化硅或粉体的纳米二氧化硅，其纳米颗粒的一次粒径为10～150nm，胶体的纳米二氧化硅的量以其中固体份二氧化硅计。加入纳米氧化硅的组分后，在煅烧过程中通过固化反应形成微纳米复合结构，纳米氧化硅由于其超高比表面积，且表面含有大量的羟基，在与陶瓷粉体固相反应时能有效降低烧结温度，同时纳米氧化硅可以使产品保持高孔隙率，实现高强度。在高强度、内部结构稳定的条件下，此纳米多孔陶瓷不易碎裂，且在使用过程中不易分离出杂质和析出重金属。
陶瓷粉体包括高岭土、硅藻土、氧化铝、氮化硅、碳化硅、石英砂、玻璃砂、黏土、长石粉中的至少一种。
造孔剂包括石墨、淀粉、面粉、豆粉、聚苯乙烯微球、聚甲基丙烯酸甲酯微球、碳酸盐、铵盐、蔗糖、纤维中的至少一种；造孔剂粒径为1～200微米。优选地，造孔剂为粒径1～20微米的鳞片状石墨。造孔剂的作用是，在纳米氧化硅保证高强度的情况下，通过调节造孔剂的添加量，使孔隙率在30～65％范围内可调。雾化芯内较高的空隙率，可使待雾化液在雾化芯的使用过程中容易渗透、传导或流通，同时不容易产生积碳而导致异味。
烧结助剂包括氧化硼、硼酸、油酸、硬脂酸、硅酸钠、氧化钙、氧化铁、氧化钛中的至少一种。
本发明的雾化芯用纳米多孔陶瓷的制备方法，包括以下步骤：
⑴按照配方称取纳米二氧化硅、陶瓷粉体、造孔剂、烧结助剂原料，置于球磨装置中混合球磨；
⑵将步骤⑴球磨后的混合料烘烤干燥，得到球磨干燥后的混合粉料；
⑶将石蜡加热至融化状态，边搅拌边加入混合粉料，加入完毕后继续搅拌1～8h，得到石蜡浆料；
⑷将石蜡浆料注入预先准备的模具中，冷却成型，脱模得到蜡模；
⑸将蜡模预加热进行除蜡，得到除蜡样；
⑹将除蜡样进行烧结，烧结过程包括升温、保温、降温，得到纳米多孔陶瓷。
另外，步骤⑴球磨机转速为150～500rpm，球磨时间为1～10h，磨料直径为1～50mm。
另外，步骤⑵烘烤干燥温度为60～150℃，干燥时间为至少1h；石蜡熔点为50～120℃，石蜡的添加量为混合粉料重量的10～60％。
另外，步骤⑸除蜡温度为400～800℃，除蜡时间为2～12h。
另外，步骤⑹烧结温度为600～1500℃，升温速度1～10℃/min，保温时间为2～12h。
另外，步骤⑹烧结过程在保护气氛下进行，保护气氛为还原性氢气气氛、惰性气氛中的一种或多种。因为单独陶瓷烧结可在空气气氛下进行，如果采用一体式烧结的金属电阻丝加热，为防止金属电阻丝在烧结过程中氧化，则需要在保护气氛下进行烧结，保护气氛可为还原性氢气气氛、惰性气氛、惰性气氛包括氮气、氩气中的一种或多种，烧结气氛不影响本发明纳米多孔陶瓷材料性能。
实施例一
具体地，本发明实施例的雾化芯用纳米多孔陶瓷，按重量份包括以下组分：纳米氧化硅15份，高岭土60份，粒径2微米的鳞片状石墨20份，硅酸钠4份，油酸1份。
实施例二
具体地，本发明实施例的雾化芯用纳米多孔陶瓷的制备方法，包括以下步骤：
⑴按照重量份称取15％的纳米二氧化硅，60％的高岭土，20％的造孔剂，4％的硅酸钠，和1％的油酸；其中，纳米二氧化硅为粒径150nm的硅溶胶，高岭土的目数为1000目，造孔剂为粒径2微米的鳞片状石墨，将称好的上述组分置于球磨装置中进行混合、球磨，球磨机转速350rpm，球磨时间10h，磨料直径为10mm；
⑵将步骤⑴中球磨好的混合料在60℃烘箱烘烤12h，得到球磨干燥后的混合粉料；
⑶称取按步骤⑵混合粉料总重量40％计算的石蜡，石蜡熔点为60℃，将石蜡加热至融化状态，边搅拌边加入上述混合粉料，加入完毕后继续搅拌并以65℃混炼6h，得到石蜡浆料；
⑷将上述石蜡浆料注入预先准备的模具中，冷却成型，脱模得到蜡模；
⑸将蜡模置于空气气氛条件的炉中加热至400℃进行除蜡，除蜡时间为6h，得到除蜡样；
⑹将上述除蜡样置于空气气氛条件的炉中进行烧结，烧结温度为950℃，升温速度为3℃/min，保温时间为4h，然后降至常温后得到纳米多孔陶瓷。
对比例：
本对比例与实施例一或实施例二的区别在于：
纳米二氧化硅15份替换为目数为1000目的石英砂15份，该石英砂为不规则分布的微米级氧化硅。
将实施例一或实施例二和对比例制得的多孔陶瓷基体按照多孔陶瓷抗压强度试验方法国标进行测定，测试结果如下表：
抗压强度/MPa
实施例一或二 22.4
对比例 14.5
由上述数据可知，对比例中采用同等量的石英砂替代纳米二氧化硅，总体材料的成分完全相同，由单分散的纳米二氧化硅替换为不规则分布的微米级氧化硅，制备的多孔陶瓷强度明显下降，说明纳米氧化硅在烧结过程中活性更强，经过固相反应后得到的陶瓷结构稳定。
以上所述仅为本发明的较佳实施例，凡依本发明权利要求范围所做的均等变化与修饰，皆应属本发明权利要求的涵盖范围。

Claims (9)

1.一种雾化芯用纳米多孔陶瓷，其特征在于，按重量份由以下组分组成：纳米氧化硅5～40份，微米级的陶瓷粉体20～70份，造孔剂5～30份，烧结助剂1～20份；所述纳米氧化硅包括胶体的纳米二氧化硅或粉体的纳米二氧化硅，所述纳米氧化硅的纳米颗粒的一次粒径为10～150nm，胶体的纳米二氧化硅的量以其中固体份二氧化硅计；所述陶瓷粉体为高岭土、硅藻土、氧化铝、氮化硅、碳化硅、石英砂、玻璃砂、黏土、长石粉中的至少一种；所述烧结助剂为氧化硼、硼酸、油酸、硬脂酸、硅酸钠、氧化钙、氧化铁、氧化钛中的至少一种。
2.根据权利要求1所述雾化芯用纳米多孔陶瓷，其特征在于，所述造孔剂为石墨、淀粉、面粉、豆粉、聚苯乙烯微球、聚甲基丙烯酸甲酯微球、碳酸盐、铵盐、蔗糖、纤维中的至少一种，所述造孔剂粒径为1～200微米。
3.根据权利要求2所述雾化芯用纳米多孔陶瓷，其特征在于，所述造孔剂为粒径1～20微米的鳞片状石墨。
4.一种根据权利要求1所述雾化芯用纳米多孔陶瓷的制备方法，其特征在于，包括以下步骤：
⑴按照配方称取纳米二氧化硅、微米级的陶瓷粉体、造孔剂、烧结助剂原料，置于球磨装置中混合球磨；
⑵将步骤⑴球磨后的混合料烘烤干燥，得到球磨干燥后的混合粉料；
⑶将石蜡加热至融化状态，边搅拌边加入所述混合粉料，加入完毕后继续搅拌1～8h，得到石蜡浆料；
⑷将所述石蜡浆料注入预先准备的模具中，冷却成型，脱模得到蜡模；
⑸将所述蜡模预加热进行除蜡，得到除蜡样；
⑹将所述除蜡样进行烧结，烧结过程包括升温、保温、降温，得到纳米多孔陶瓷。
5.根据权利要4所述雾化芯用纳米多孔陶瓷的制备方法，其特征在于，步骤⑴所述球磨装置转速为150～500rpm，球磨时间为1～10h，磨料直径为1～50mm。
6.根据权利要求4所述雾化芯用纳米多孔陶瓷的制备方法，其特征在于，步骤⑵所述烘烤干燥温度为60～150℃，干燥时间为至少1h；步骤⑶所述石蜡熔点为50～120℃，石蜡的添加量为混合粉料重量的10～60％。
7.根据权利要求4所述雾化芯用纳米多孔陶瓷的制备方法，其特征在于，步骤⑸所述除蜡温度为400～800℃，除蜡时间为2～12h。
8.根据权利要求4所述雾化芯用纳米多孔陶瓷的制备方法，其特征在于，步骤⑹所述烧结温度为600～1500℃，升温速度1～10℃/min，保温时间为2～12h。
9.根据权利要求4所述雾化芯用纳米多孔陶瓷的制备方法，其特征在于，步骤⑹所述烧结过程在保护气氛下进行，所述保护气氛为还原性氢气气氛、惰性气氛中的一种或多种。
CN202011561865.7A 2020-12-18 2020-12-25 雾化芯用纳米多孔陶瓷及其制备方法 Active CN112592200B (zh)

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CN115215676A (zh) * 2021-04-15 2022-10-21 深圳市吉迩科技有限公司 多孔陶瓷材料、制作方法、多孔陶瓷及应用
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CN114195493A (zh) * 2021-12-09 2022-03-18 深圳市基克纳科技有限公司 一种多孔陶瓷雾化芯的制备方法、陶瓷雾化芯及其应用
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CN114478052A (zh) * 2022-01-17 2022-05-13 刘松青 一种高强度电子烟陶瓷雾化芯制备方法
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