CN114477971B - 一种电子烟用微孔陶瓷及其制备方法 - Google Patents

一种电子烟用微孔陶瓷及其制备方法 Download PDF

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CN114477971B
CN114477971B CN202210304132.8A CN202210304132A CN114477971B CN 114477971 B CN114477971 B CN 114477971B CN 202210304132 A CN202210304132 A CN 202210304132A CN 114477971 B CN114477971 B CN 114477971B
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张南泉
张伟群
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Guizhou Qunhua Jiujiu Special Ceramic Technology Co ltd
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Abstract

本发明涉及非金属复合材料领域，具体为一种电子烟用微孔陶瓷及其制备方法，包括位于内部的陶瓷微孔层和位于外部的陶瓷防护层，所述陶瓷微孔层的体积密度为1.10‑1.20g/cm3，孔尺寸分布范围为0.01‑1.5μm，导热系数为8‑10W/m·K，所述陶瓷防护层的导热系数为0.05‑0.1W/m·K，抗压强度为90‑110MPa，其中，陶瓷微孔层具有较低的体积密度和较高的导热系数，对于烟油具有良好的吸油和锁油效果，而陶瓷防护层具有较低的导热系数和较高的抗压强度，位于陶瓷微孔层外侧，可以保护内部，且可以起到良好的隔热、防冲击效果。

Description

一种电子烟用微孔陶瓷及其制备方法
技术领域
本发明涉及非金属复合材料领域，具体为一种电子烟用微孔陶瓷及其制备方法。
背景技术
微孔陶瓷作为一种具有均匀微气孔结构的陶瓷，是一种新型陶瓷材料，也是一种功能型的结构陶瓷，其孔径一般为微米级或亚微米级，是肉眼基本看不见的。但微孔陶瓷在日常生活应用较为普遍，常被用于作为电子烟里的雾化芯，目前电子烟中微孔陶瓷的热导率低，升温均匀度差，影响口感，而且孔多通过造孔剂法制出，多为闭气孔，连通性较差，导致吸油、导油、雾化效果不好。
发明内容
发明目的：针对上述技术问题，本发明提出了一种电子烟用微孔陶瓷及其制备方法。
所采用的技术方案如下：
一种电子烟用微孔陶瓷，包括位于内部的陶瓷微孔层和位于外部的陶瓷防护层，所述陶瓷微孔层的体积密度为1.10-1.20g/cm3，孔尺寸分布范围为0.01-1.5μm，导热系数为8-10W/m·K，所述陶瓷防护层的导热系数为0.05-0.1W/m·K，抗压强度为90-110MPa。
进一步地，所述陶瓷微孔层的厚度为5-10μm。
进一步地，所述陶瓷防护层的厚度为10-50μm。
进一步地，以重量份数计，制备所述陶瓷微孔层的原料包括：
氧化铝30-40份、蓝晶石15-25份、钠长石5-10份、凹凸棒石粘土5-10份、氧化锂1-2份、二氧化钛5-10份、纳米羟基磷灰石5-10份、炭黑45-55份、烧结助剂1-2份。
进一步地，所述烧结助剂为玻璃粉。
进一步地，所述烧结助剂为Bi2O3-SiO2-B2O3玻璃粉。
进一步地，以重量份数计，制备所述陶瓷防护层的原料包括：
九水合硝酸铝20-25份、正硅酸乙酯28-32份、钇稳定氧化锆纳米晶5-10份、无水乙醇300-400份。
本发明还提供了一种电子烟用微孔陶瓷的制备方法：
分别获取陶瓷微孔层浆料和陶瓷防护层浆料，分别将所述陶瓷微孔层浆料、陶瓷防护层浆料进行流延成型，得到陶瓷微孔层和陶瓷防护层，将陶瓷微孔层烧结后经盐酸溶液负压浸渍后烘干，与陶瓷防护层层叠后干压成型并烧结，即可得到所述电子烟用微孔陶瓷。
进一步地，所述电子烟用微孔陶瓷的制备方法，具体包括以下步骤：
S1：将二氧化钛、炭黑预先球磨5-10h后与氧化铝、蓝晶石、钠长石、凹凸棒石粘土、氧化锂、纳米羟基磷灰石、烧结助剂混合均匀，球磨5-10h，加入流延剂，继续球磨5-10h，制成陶瓷微孔层浆料；
S2：将无水乙醇分为两份，将九水合硝酸铝加入第一份无水乙醇中，升温至回流20-25h后加入钇稳定氧化锆纳米晶超声振荡混合均匀后待用，再将正硅酸乙酯加入第二份无水乙醇中，40-45℃搅拌2-4h后加入，保持回流反应4-8d后得到溶胶，所得溶胶于60-70℃老化8-15h后于100-120℃干燥2-4d后研磨成粉体，先于600-800℃保温10-15h，再于1200-1400℃保温2-4h，恢复室温后加入流延剂中，球磨15-20h，制成陶瓷防护层浆料；
S3：通过流延成型，得到陶瓷微孔层和陶瓷防护层，将得到的陶瓷微孔层于1750-1800℃烧结1.5-2h，再置于盐酸溶液中负压浸渍10-15h后烘干，与陶瓷防护层层叠，并于温度为90-100℃，10-20MPa下干压成型，最后先于450-500℃排胶30-60min，再于1200-1500℃烧结1-2h即可得到所述电子烟用微孔陶瓷。
进一步地，以重量份数计，所述流延剂包括以下组成成分：
三油酸甘油酯3-5份、鲱鱼油1-2份、聚乙烯醇缩丁醛6-10份、邻苯二甲酸二丁酯0.1-0.5份、邻苯二甲酸二辛酯0.1-0.5份、乙醇200-250份、水100-120份。
本发明的有益效果：
本发明提供了一种电子烟用微孔陶瓷，包括位于内部的陶瓷微孔层和位于外部的陶瓷防护层，其中，陶瓷微孔层具有较低的体积密度和较高的导热系数，孔尺寸分布范围为0.01-1.5μm，且多为开孔和贯穿孔，对于烟油具有良好的吸油和锁油效果，可实现对雾化器烟油的顺畅供给和吸附锁油，有效降低干烧风险，加热后，微孔陶瓷温度迅速升高并被烟油充分浸润，每一滴烟油都能够通过微孔充分加热，确保使用者口感，而陶瓷防护层具有较低的导热系数和较高的抗压强度，位于陶瓷微孔层外侧，可以保护内部，且可以起到良好的隔热、防冲击效果。
附图说明
图1为本发明电子烟用微孔陶瓷的结构示意图；
图2为本发明实施例1中陶瓷微孔层的微观结构图；
图中标号分别代表：
1-陶瓷防护；2-陶瓷微孔层。
具体实施方式
实施例中未注明具体条件者，按照常规条件或制造商建议的条件进行。所用试剂或仪器未注明生产厂商者，均为可以通过市售购买获得的常规产品。
实施例1：
一种电子烟用微孔陶瓷的制备方法：
将45g三油酸甘油酯、15g鲱鱼油、80g聚乙烯醇缩丁醛、2g邻苯二甲酸二丁酯、1g邻苯二甲酸二辛酯、2000g乙醇、1200g水混合搅拌均匀得到流延剂，将10g二氧化钛、50g炭黑预先球磨10h后与40g氧化铝、20g蓝晶石、5g钠长石、5g凹凸棒石粘土、1g氧化锂、10g纳米羟基磷灰石、1g Bi2O3-SiO2-B2O3玻璃粉混合均匀，球磨10h，加入800mL流延剂，继续球磨10h，脱泡，制成陶瓷微孔层浆料，将600g无水乙醇分为两份，将40g九水合硝酸铝加入第一份300g无水乙醇中，升温至回流25h后加入15g钇稳定氧化锆纳米晶超声振荡混合均匀后待用，再将60g正硅酸乙酯加入第二份300g无水乙醇中，45℃搅拌2h后加入，保持回流反应6d后得到溶胶，所得溶胶于60℃老化12h后于120℃干燥2d后研磨成粉体，先于600℃保温15h，再于1300℃保温4h，恢复室温后加入300mL流延剂中，球磨20h，脱泡，制成陶瓷防护层浆料，分别将陶瓷微孔层浆料、陶瓷防护层浆料加入KY-CAM流延机中通过流延成型，得到陶瓷微孔层(2)和陶瓷防护层(1)，将得到的陶瓷微孔层(2)于1800℃烧结1.5h，再置于质量分数10％的盐酸溶液中真空度为0.04MPa下负压浸渍15h后水洗、烘干，将其与陶瓷防护层(1)层叠，并于温度为90℃，15MPa下干压成型，所得坯体先于480℃排胶50min，再于1350℃烧结2h即可得到所述电子烟用微孔陶瓷。
实施例2：
一种电子烟用微孔陶瓷的制备方法：
将50g三油酸甘油酯、20g鲱鱼油、100g聚乙烯醇缩丁醛、5g邻苯二甲酸二丁酯、5g邻苯二甲酸二辛酯、2500g乙醇、1200g水混合搅拌均匀得到流延剂，将10g二氧化钛、55g炭黑预先球磨10h后与40g氧化铝、25g蓝晶石、10g钠长石、10g凹凸棒石粘土、2g氧化锂、10g纳米羟基磷灰石、2g Bi2O3-SiO2-B2O3玻璃粉混合均匀，球磨10h，加入800mL流延剂，继续球磨10h，脱泡，制成陶瓷微孔层浆料，将600g无水乙醇分为两份，将50g九水合硝酸铝加入第一份300g无水乙醇中，升温至回流25h后加入20g钇稳定氧化锆纳米晶超声振荡混合均匀后待用，再将64g正硅酸乙酯加入第二份300g无水乙醇中，45℃搅拌4h后加入，保持回流反应8d后得到溶胶，所得溶胶于70℃老化15h后于120℃干燥4d后研磨成粉体，先于800℃保温15h，再于1400℃保温4h，恢复室温后加入300mL流延剂中，球磨20h，脱泡，制成陶瓷防护层浆料，分别将陶瓷微孔层浆料、陶瓷防护层浆料加入KY-CAM流延机中通过流延成型，得到陶瓷微孔层(2)和陶瓷防护层(1)，将得到的陶瓷微孔层(2)于1800℃烧结2h，再置于质量分数10％的盐酸溶液中真空度为0.04MPa下负压浸渍15h后水洗、烘干，将其与陶瓷防护层(1)层叠，并于温度为100℃，20MPa下干压成型，所得坯体先于500℃排胶60min，再于1500℃烧结2h即可得到所述电子烟用微孔陶瓷。
实施例3：
一种电子烟用微孔陶瓷的制备方法：
将30g三油酸甘油酯、10g鲱鱼油、60g聚乙烯醇缩丁醛、1g邻苯二甲酸二丁酯、1g邻苯二甲酸二辛酯、2000g乙醇、1000g水混合搅拌均匀得到流延剂，将5g二氧化钛、45g炭黑预先球磨5h后与30g氧化铝、15g蓝晶石、5g钠长石、5g凹凸棒石粘土、1g氧化锂、5g纳米羟基磷灰石、1g Bi2O3-SiO2-B2O3玻璃粉混合均匀，球磨5h，加入800mL流延剂，继续球磨5h，脱泡，制成陶瓷微孔层浆料，将600g无水乙醇分为两份，将40g九水合硝酸铝加入第一份300g无水乙醇中，升温至回流20h后加入10g钇稳定氧化锆纳米晶超声振荡混合均匀后待用，再将56g正硅酸乙酯加入第二份300g无水乙醇中，40℃搅拌2h后加入，保持回流反应4d后得到溶胶，所得溶胶于60℃老化8h后于100℃干燥2d后研磨成粉体，先于600℃保温10h，再于1200℃保温2h，恢复室温后加入300mL流延剂中，球磨15h，脱泡，制成陶瓷防护层浆料，分别将陶瓷微孔层浆料、陶瓷防护层浆料加入KY-CAM流延机中通过流延成型，得到陶瓷微孔层(2)和陶瓷防护层(1)，将得到的陶瓷微孔层(2)于1750℃烧结1.5h，再置于质量分数10％的盐酸溶液中真空度为0.04MPa下负压浸渍10h后水洗、烘干，将其与陶瓷防护层(1)层叠，并于温度为90℃，10MPa下干压成型，所得坯体先于450℃排胶30min，再于1200℃烧结1h即可得到所述电子烟用微孔陶瓷。
实施例4：
一种电子烟用微孔陶瓷的制备方法：
将50g三油酸甘油酯、10g鲱鱼油、100g聚乙烯醇缩丁醛、1g邻苯二甲酸二丁酯、5g邻苯二甲酸二辛酯、2000g乙醇、1200g水混合搅拌均匀得到流延剂，将5g二氧化钛、55g炭黑预先球磨5h后与40g氧化铝、15g蓝晶石、10g钠长石、5g凹凸棒石粘土、2g氧化锂、5g纳米羟基磷灰石、2g Bi2O3-SiO2-B2O3玻璃粉混合均匀，球磨5h，加入800mL流延剂，继续球磨10h，脱泡，制成陶瓷微孔层浆料，将600g无水乙醇分为两份，将40g九水合硝酸铝加入第一份300g无水乙醇中，升温至回流25h后加入10g钇稳定氧化锆纳米晶超声振荡混合均匀后待用，再将64g正硅酸乙酯加入第二份300g无水乙醇中，40℃搅拌4h后加入，保持回流反应4d后得到溶胶，所得溶胶于70℃老化8h后于120℃干燥2d后研磨成粉体，先于800℃保温10h，再于1400℃保温2h，恢复室温后加入300mL流延剂中，球磨20h，脱泡，制成陶瓷防护层浆料，分别将陶瓷微孔层浆料、陶瓷防护层浆料加入KY-CAM流延机中通过流延成型，得到陶瓷微孔层(2)和陶瓷防护层(1)，将得到的陶瓷微孔层(2)于1750℃烧结2h，再置于质量分数10％的盐酸溶液中真空度为0.04MPa下负压浸渍10h后水洗、烘干，将其与陶瓷防护层(1)层叠，并于温度为100℃，10MPa下干压成型，所得坯体先于500℃排胶30min，再于1500℃烧结1h即可得到所述电子烟用微孔陶瓷。
实施例5：
一种电子烟用微孔陶瓷的制备方法：
将30g三油酸甘油酯、20g鲱鱼油、60g聚乙烯醇缩丁醛、5g邻苯二甲酸二丁酯、1g邻苯二甲酸二辛酯、2500g乙醇、1000g水混合搅拌均匀得到流延剂，将10g二氧化钛、45g炭黑预先球磨10h后与30g氧化铝、25g蓝晶石、5g钠长石、10g凹凸棒石粘土、1g氧化锂、10g纳米羟基磷灰石、1g Bi2O3-SiO2-B2O3玻璃粉混合均匀，球磨10h，加入800mL流延剂，继续球磨5h，脱泡，制成陶瓷微孔层浆料，将600g无水乙醇分为两份，将50g九水合硝酸铝加入第一份300g无水乙醇中，升温至回流20h后加入20g钇稳定氧化锆纳米晶超声振荡混合均匀后待用，再将56g正硅酸乙酯加入第二份300g无水乙醇中，45℃搅拌2h后加入，保持回流反应8d后得到溶胶，所得溶胶于60℃老化15h后于100℃干燥4d后研磨成粉体，先于700℃保温15h，再于1200℃保温4h，恢复室温后加入300mL流延剂中，球磨15h，脱泡，制成陶瓷防护层浆料，分别将陶瓷微孔层浆料、陶瓷防护层浆料加入KY-CAM流延机中通过流延成型，得到陶瓷微孔层(2)和陶瓷防护层(1)，将得到的陶瓷微孔层(2)于1800℃烧结1.5h，再置于质量分数10％的盐酸溶液中真空度为0.04MPa下负压浸渍15h后水洗、烘干，将其与陶瓷防护层(1)层叠，并于温度为90℃，20MPa下干压成型，所得坯体先于450℃排胶60min，再于1300℃烧结2h即可得到所述电子烟用微孔陶瓷。
对比例1
对比例1与实施例1基本相同，区别在于，不加入Bi2O3-SiO2-B2O3玻璃粉。
对比例2
对比例2与实施例1基本相同，区别在于，钇稳定氧化锆纳米晶钇稳定氧化锆纳米晶。
性能测试：
①分别将本发明实施例1-5及对比例1-2所制备的电子烟用微孔陶瓷作为试样进行测试，测试结果如下表1所示：
表1：
Figure BDA0003564160310000081
.由上表1可知，本发明所制备的电子烟用微孔陶瓷中陶瓷微孔层具有较低的体积密度和较高的导热系数，而陶瓷防护层具有较低的导热系数和较高的抗压强度，可以起到较好的隔热、防护效果。
②将本发明实施例1-5制备的电子烟用微孔陶瓷和对比例1制备的电子烟用微孔陶瓷放于相同体积的烟油内，测量5min内，烟油被吸收的量，记为吸油率，再将上述电子烟用微孔陶瓷取出，测量5min内，烟油的渗出量，记为渗油率，测试结果如表2所示：
吸油率＝[(m2-m1)/m1]*100％
渗油率＝[(m2-m3)/m3]*100％
m1为微孔陶瓷质量，m2为吸收烟油后微孔陶瓷质量，m3为渗出烟油后微孔陶瓷质量。
表2：
吸油率/％ 渗油率/％
实施例1 56.2 1.3
实施例2 54.8 1.5
实施例3 54.3 1.6
实施例4 55.4 1.5
实施例5 55.9 1.4
对比例1 46.7 3.3
由上表2可知，本发明所制备的电子烟用微孔陶瓷对于烟油具有良好的吸油和锁油效果。
以上实施例仅用以说明本发明的技术方案，而非对其限制；尽管参照前述实施例对本发明进行了详细的说明，本领域的普通技术人员应当理解：其依然可以对前述各实施例所记载的技术方案进行修改，或者对其中部分技术特征进行等同替换；而这些修改或者替换，并不使相应技术方案的本质脱离本发明各实施例技术方案的精神和范围。

Claims (4)

1.一种电子烟用微孔陶瓷，其特征在于，包括位于内部的陶瓷微孔层和位于外部的陶瓷防护层，所述陶瓷微孔层的体积密度为1.10-1.20g/cm3，孔尺寸分布范围为0.01-1.5μm，导热系数为8-10W/m·K，所述陶瓷防护层的导热系数为0.05-0.1W/m·K，抗压强度为90-110MPa；
以重量份数计，制备所述陶瓷微孔层的原料包括：
氧化铝30-40份、蓝晶石15-25份、钠长石5-10份、凹凸棒石粘土5-10份、氧化锂1-2份、二氧化钛5-10份、纳米羟基磷灰石5-10份、炭黑45-55份、烧结助剂1-2份；
以重量份数计，制备所述陶瓷防护层的原料包括：
九水合硝酸铝20-25份、正硅酸乙酯28-32份、钇稳定氧化锆纳米晶5-10份、无水乙醇300-400份；
所述烧结助剂为Bi2O3-SiO2-B2O3玻璃粉；
上述电子烟用微孔陶瓷的制备方法，具体包括以下步骤：
S1：将二氧化钛、炭黑预先球磨5-10h后与氧化铝、蓝晶石、钠长石、凹凸棒石粘土、氧化锂、纳米羟基磷灰石、烧结助剂混合均匀，球磨5-10h，加入流延剂，继续球磨5-10h，制成陶瓷微孔层浆料；
S2：将无水乙醇分为两份，将九水合硝酸铝加入第一份无水乙醇中，升温至回流20-25h后加入钇稳定氧化锆纳米晶超声振荡混合均匀后待用，再将正硅酸乙酯加入第二份无水乙醇中，40-45℃搅拌2-4h后加入，保持回流反应4-8d后得到溶胶，所得溶胶于60-70℃老化8-15h后于100-120℃干燥2-4d后研磨成粉体，先于600-800℃保温10-15h，再于1200-1400℃保温2-4h，恢复室温后加入流延剂中，球磨15-20h，制成陶瓷防护层浆料；
S3：通过流延成型，得到陶瓷微孔层和陶瓷防护层，将得到的陶瓷微孔层于1750-1800℃烧结1.5-2h，再置于盐酸溶液中负压浸渍10-15h后烘干，与陶瓷防护层层叠，并于温度为90-100℃，10-20MPa下干压成型，最后先于450-500℃排胶30-60min，再于1200-1500℃烧结1-2h即可得到所述电子烟用微孔陶瓷。
2.如权利要求1所述的电子烟用微孔陶瓷，其特征在于，所述陶瓷微孔层的厚度为5-10μm。
3.如权利要求1所述的电子烟用微孔陶瓷，其特征在于，所述陶瓷防护层的厚度为10-50μm。
4.如权利要求1所述的电子烟用微孔陶瓷，其特征在于，以重量份数计，所述流延剂包括以下组成成分：
三油酸甘油酯3-5份、鲱鱼油1-2份、聚乙烯醇缩丁醛6-10份、邻苯二甲酸二丁酯0.1-0.5份、邻苯二甲酸二辛酯0.1-0.5份、乙醇200-250份、水100-120份。
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