CN116477966A - 一种不掉粉的羟基磷灰石基多孔陶瓷的制备方法 - Google Patents
一种不掉粉的羟基磷灰石基多孔陶瓷的制备方法 Download PDFInfo
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Abstract
本发明涉及一种不掉粉的羟基磷灰石基多孔陶瓷的制备方法，按质量比羟基磷灰石粉末:拟薄水铝石粉末:偏铁酸钠:淀粉:水＝2:(0.15‑0.25):(0.28‑0.46):(0.1‑0.15):(2.4‑2.8)将上述各物质充分混合成膏状物料，然后将所述膏状物料成型为生坯体，然后将所述生坯体在空气气氛下从环境温度升温至800～900℃并在800～900℃下预烧1.5～2h，接着在空气气氛下升温至1100‑1160℃下烧结4～6小时，得到所述不掉粉(3000次抽吸循环后重量减少百分比小于0.25％)的羟基磷灰石基多孔陶瓷。
Description
技术领域
本发明属于电子烟雾化器具领域，特别涉及一种不掉粉的羟基磷灰石基多孔陶瓷的制备方法。
背景技术
电子烟中的陶瓷芯雾化器多采用多孔陶瓷体搭载金属发热片的组合方式，其中多孔陶瓷体靠其多孔导油性能将电子烟的储油仓中的烟油传递给金属发热片，金属发热片则通电后靠电阻发热来将烟油雾化，雾化产生的烟雾还可以通过多孔陶瓷的孔隙向外扩散，最终汇总到烟嘴中供用户抽吸。
现有的多孔陶瓷体多为氧化铝陶瓷，例如氧化铝陶瓷制备的加热片、加热棒、或者雾化芯，其具有一定的刚度、不易弯折，导热效果好、绝缘性好。但是，实践中发现氧化铝陶瓷发热体存在掉粉现象，即加热烟油一段时间后，氧化铝陶瓷会有粉体脱落现象，据报道氧化铝多孔陶瓷雾化芯样品在长期抽吸前后重量减小百分比(即掉粉率)可高达1.32％～1.76％。这对于电子烟来说，是极大的弊端。因为，用户依靠抽吸作用抽吸电子烟产生的烟雾，若氧化铝陶瓷出现粉体脱落，则粉体会随着烟雾进入用户的呼吸道和肺部，会极大影响用户身体健康。为解决掉粉问题，我司曾经申请了专利202011134813.1，提出一种羟基磷灰石基多孔陶瓷的技术方案，可以在抽吸3000次循环后将掉粉率控制在0.6％以下，但人们希望能继续降低掉粉率。
为此，提出本发明。
发明内容
本发明提供了一种不掉粉的羟基磷灰石基多孔陶瓷的制备方法，按质量比羟基磷灰石粉末:拟薄水铝石粉末:偏铁酸钠:淀粉:水＝2:(0.15-0.25):(0.28-0.46):(0.1-0.15):(2.4-2.8)将上述各物质充分混合成膏状物料，然后将所述膏状物料成型为生坯体，然后将所述生坯体在空气气氛下从环境温度升温至800～900℃并在800～900℃下预烧1.5～2h，接着在空气气氛下升温至1100-1160℃下烧结4～6小时，得到所述不掉粉的羟基磷灰石基多孔陶瓷。
优选地，所述膏状物料中还含有分散剂六偏磷酸钠，其量占所述膏状物料的0.8-1.2wt％，可用于将粉体物料均匀分散于水中，避免出现化不开的粉体团块。还可以使用诸如聚丙烯酸钠等其他分散剂来代替六偏磷酸钠。分散剂也可以不加。
优选地，所述拟薄水铝石的粒径为100目～625目，所述羟基磷灰石粒径为100目～625目，所述淀粉的粒径为100目～625目。
本发明中，拟薄水铝石(分子式为AlOOH)起到无机粘合剂的作用，用于将各固体物料与水制成具有形状自维持性的粘稠的膏状物料，以便使成型后的生坯体具有固定的预设几何形状。
本发明的方法中，将所述生坯体在空气气氛下从环境温度升温至800～900℃并在800～900℃下预烧1.5～2h，是为了脱除膏状物料中的游离水以及烧毁其中的淀粉以及任何所含的其他有机物质，则原来游离水和淀粉以及其他有机物质所占据的空间被空出来，形成孔隙。在该过程末段，800～900℃的温度也足以让颗粒间接触点处形成预烧结点，则颗粒间架桥作用使得孔隙被保持，为下一步更高温度下烧结创造条件。
然后在空气气氛下升温至1100～1160℃下烧结4-6小时，羟基磷灰石颗粒间接触点及附近材料会在该温度下局部熔化为粘稠熔融料而将众多颗粒彼此连接起来，冷却后则形成多孔陶瓷体。
发明人意外发现，拟薄水铝石不仅起到无机粘合剂的作用，向生坯中加入拟薄水铝石粉末和偏铁酸钠(分子式为NaFeO2)这个特定组合后，再经预烧和烧结，还能得到几乎不掉粉的羟基磷灰石基多孔陶瓷，发明人根据后续实施例实验猜测其可能的原因有二：一是因为偏铁酸钠中的钠元素在高温下能被液化并在表面张力作用下趋于汇集到颗粒间的预烧结点处，再冷却后又固化，对烧结点起到了结构强化作用，防止颗粒脱落。二是薄水铝石粉末和偏铁酸钠粉末在高温下预烧和烧结过程中产生的新生态α-Al2O3与新生态Fe2O3可能产生了某种金属氧化物固溶体，起到了辅助烧结和强化多孔体结构的作用。
附图说明
无。
具体实施方式
下面通过具体实施方式进一步说明本发明的内容。
实施例1
取市售100目羟基磷灰石粉末200g、市售100目拟薄水铝石粉末15g、市售100目偏铁酸钠28g、100目小麦淀粉10g和240g自来水均匀混合后配制成粘稠膏状混合物料，通过模具填充法制备成圆柱形生坯10个。然后按下述过程进行程序升温：将各个生坯体放入马弗炉中，从室温下升温到900℃并在900℃下保持1.5h，然后以2℃/秒的升温速度升温到1100℃并保持在该温度下烧结6h，然后自然冷却到室温，得到羟基磷灰石基多孔陶瓷。向该多孔陶瓷表面贴附铂合金电阻发热片，形成1#陶瓷雾化芯。
实施例2
取市售625目羟基磷灰石粉末200g、市售625目拟薄水铝石粉末25g、市售625目偏铁酸钠46g、625目小麦淀粉15g和280g自来水均匀混合后配制成粘稠膏状混合物料，通过模具填充法制备成圆柱形生坯10个。然后按下述过程进行程序升温：将各个生坯体放入马弗炉中，从室温下升温到800℃并在800℃下保持2h，然后以2℃/秒的升温速度升温到1160℃并保持在该温度下烧结4h，然后自然冷却到室温，得到羟基磷灰石基多孔陶瓷。向该多孔陶瓷表面贴附与实施例1相同的铂合金电阻发热片，形成2#陶瓷雾化芯。
对比例1
取市售100目羟基磷灰石粉末200g、市售100目α-Al2O3粉末12.75g、市售100目Fe2O3粉末20.2g、100目小麦淀粉10g和240g自来水均匀混合后配制成粘稠膏状混合物料，通过模具填充法制备成圆柱形生坯10个。然后按下述过程进行程序升温：将各个生坯体放入马弗炉中，从室温下升温到900℃并在900℃下保持1.5h，然后以2℃/秒的升温速度升温到1100℃并保持在该温度下烧结6h，然后自然冷却到室温，得到羟基磷灰石基多孔陶瓷。向该多孔陶瓷表面贴附与实施例1相同的铂合金电阻发热片，形成3#陶瓷雾化芯。
实施例3
该实施例进行掉粉率测试。
将·上述1#、2#和3#陶瓷雾化芯各10个样品，分别装配到同款电子烟具中，按照同样的加热程序(15秒内从室温加热到220℃并在220℃下长期保持)抽吸同样配方的电子烟烟油(主要成分是甘油、水、烟碱和薄荷口味香料)3000次，考察其重量变化比及(抽吸前重量-抽吸后重量)/抽吸前重量*100，如下表所示：
从上表1，可以发现，3000次抽吸循环后，本发明的1#和2#羟基磷灰石基多孔陶瓷雾化芯样品重量减小百分比(即掉粉率)均在0.25％以下，大大低于专利202011134813.1中所示的约0.6％的掉粉率，这在行业内几乎可以被认为是不掉粉。3#样品则掉粉率介于0.78％至0.99％之间，比纯羟基磷灰石基多孔陶瓷的掉粉率0.6％还要高，可见虽然3#配方中也加入了α-Al2O3和Fe2O3粉末，但它们是原始加入的而不是在高温下新生成的新生态，可能彼此反应性不够，故没有起到减少掉粉率的作用，反倒增加了掉粉率。
以上所述，仅为本发明的具体实施方式，但本发明的保护范围并不局限于此，任何熟悉本技术领域的技术人员在本发明揭露的技术范围内，可轻易想到变化或替换，都应涵盖在本发明的保护范围之内。因此，本发明的保护范围应以权利要求的保护范围为准。
Claims (3)
1.一种不掉粉的羟基磷灰石基多孔陶瓷的制备方法，其特征在于，按质量比羟基磷灰石粉末:拟薄水铝石粉末:偏铁酸钠:淀粉:水＝2:(0.15-0.25):(0.28-0.46):(0.1-0.15):(2.4-2.8)将上述各物质充分混合成膏状物料，然后将所述膏状物料成型为生坯体，然后将所述生坯体在空气气氛下从环境温度升温至800～900℃并在800～900℃下预烧1.5～2h，接着在空气气氛下升温至1100-1160℃下烧结4～6小时，得到所述不掉粉的羟基磷灰石基多孔陶瓷。
2.根据权利要求1所述的制备方法，其特征在于，所述膏状物料中还含有分散剂六偏磷酸钠，其量占所述膏状物料的0.8-1.2wt％。
3.根据权利要求1所述的制备方法，其特征在于，所述拟薄水铝石的粒径为100目～625目，所述羟基磷灰石粒径为100目～625目，所述淀粉的粒径为100目～625目。
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