CN109095948B - 一种利用中空微球制备具有连通孔壁泡沫陶瓷的方法 - Google Patents
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Abstract
本发明开发了一种利用中空微球制备具有连通孔壁泡沫陶瓷的方法，该方法包括如下步骤：以陶瓷粉和中空微球为原料，配制总固相含量为20～50wt％的水基浆料。在上述浆料中加入表面活性剂对陶瓷粉体进行疏水化修饰。通过机械搅拌方式对浆料进行发泡得到陶瓷颗粒和中空微球协同稳定的泡沫，泡沫干燥后进行烧结获得具有连通孔壁泡沫陶瓷。嵌入在孔壁上的中空微球经过烧结处理起到成孔作用，因此本发明制备的泡沫结构具有高度开孔结构，可以满足其在吸附，催化，过滤等领域的应用。
Description
技术领域
本发明属于开孔泡沫陶瓷材料技术领域，具体涉及一种利用中空微球制备具有连通孔壁泡沫陶瓷的方法。
背景技术
泡沫陶瓷结合了多孔材料和陶瓷材料的优点，具有耐高温、高气孔率、隔热、化学稳定等性能，广泛应用于流体过滤，催化剂载体，以及人工骨等领域。多孔材料的制备方法主要有有机泡沫浸渍法、添加造孔剂法、直接发泡法、固态烧结法(又称骨料堆积法)、溶胶-凝胶法、冷冻干燥法等。浆料直接发泡法相比于其它方法，更易于制备高气孔率泡沫陶瓷，制备工艺相对简单。近些年快速发展的颗粒稳定泡沫法，利用不可逆的吸附在气/液界面的陶瓷颗粒本身稳定泡沫使其可以抵制泡沫的破裂、排液、歧化、奥斯瓦尔德熟化等不稳定因素。因此该方法无需附加凝胶等方法辅助其固化，更加经济、简单。然而由于陶瓷颗粒在气/液界面的紧密组成使所获得的泡沫陶瓷为闭孔结构。所以，目前为止，直接发泡法制备的泡沫陶瓷多以孔壁为主，难以获得高度开孔的结构，这使得泡沫陶瓷只能应用在保温上，一旦孔壁结构为闭孔或者少量开孔，其透气性必然很差，即使透气也面临巨大的压阻，无法在吸附，催化，过滤，能量转换等领域应用。因此如何利用颗粒稳定泡沫法制备高度开孔的泡沫陶瓷具有重要意义。
发明内容
针对上述背景技术以及存在的问题，本发明开发了一种利用中空微球制备具有连通孔壁泡沫陶瓷的方法。本发明首次采用空心球做造孔剂，使其稳定地吸附在液膜上，通过后期烧结处理使孔壁得到开孔结构。进一步的，其制备工艺简单，成本低廉，环境友好。
本发明采用技术路线如下，一种利用中空微球制备具有连通孔壁泡沫陶瓷的方法，包括如下步骤：
(1)以陶瓷粉和中空微球为原料，配制总固相含量为20～50wt％的水基浆料。所采用材料的陶瓷粉体包括氧化铝、氧化铈、氧化锆、莫来石，其粒径范围为0.2～4.5μm。所述中空微球为无机空心球，包括玻璃基空心球，氧化硅基空心球，其烧成温度为500～900℃，粒径为10～60μm。所述水基浆料中的中空微球的含量为5～20wt％。
(2)在上述浆料中加入表面活性剂对陶瓷粉体进行疏水化修饰，表面活性剂为十二烷基硫酸钠和/或十六烷基硫酸钠，其加入量为总浆料质量的0.03～0.3wt％。
(3)通过机械搅拌方式对浆料进行发泡得到陶瓷颗粒和中空微球协同稳定的泡沫。
(4)将泡沫干燥后进行烧结，其烧结温度为1350～1600℃。
所制备获得的泡沫具有稳定性，中空微球均匀地分布在整个泡沫体系中。
本发明制备的泡沫材料具有40～200μm的一级宏孔结构，其孔壁则由空心球堆积紧密而成，孔壁具有均匀的开孔结构，开孔孔径大小为10～60μm。
本发明的有益效果是：
本方法所制备的泡沫陶瓷具有高度开孔结构，且开孔分布均匀。
该方法无需泡沫固化措施，工艺简单。
该方法每个生产环节不产生有毒、有害物质，环境友好。
嵌入在孔壁上的中空微球经过烧结处理起到成孔作用，因此本发明制备的泡沫结构具有高度开孔结构，可以满足其在吸附，催化，过滤等领域的应用。
附图说明
图1是本发明实施例所用的中空微球的微观照片。
图2是本发明实施例所用的中空微球的粒径分布。
图3是本发明实施例制备的开孔泡沫氧化铈微观照片，显示了均匀分布的开孔结构。
具体实施方式
下面结合附图和实施例对本发明进一步详细说明。
实施例1
利用中空微球制备具有连通孔壁泡沫陶瓷的方法，包括如下步骤：
(1)配制含有40wt％氧化铈和10wt％氧化硅空心微球的浆料，氧化铈平均粒径为0.32μm，氧化硅空心微球粒径主要分布在15-60μm，如图1和图2所示，其堆积密度为0.22g/cm3。
(2)在配制好的浆料中加入0.08wt％的十二烷基硫酸钠，然后调pH至6.8。
(3)利用机械搅拌机在2000rmp转速下搅拌发泡10min得到稳定的陶瓷泡沫浆料。干燥后得到干坯。
(4)坯体以3℃/min升温速率加热至1500℃，保温2h。制备得到如图3所示的开孔氧化铈泡沫陶瓷，其开孔孔径分布为10～60μm。
上述实施例对本发明的技术方案进行了详细说明。显然，本发明并不局限于所描述的实施例。基于本发明中的实施例，熟悉本技术领域的人员还可据此做出多种变化，但任何与本发明等同或相类似的变化都属于本发明保护的范围。
Claims (4)
1.一种具有连通孔壁的泡沫陶瓷，其特征在于，通过如下步骤制备：
(1)以陶瓷粉和中空微球为原料，配制总固相含量为20～50wt％的水基浆料；所述中空微球为无机空心球，包括玻璃基空心球或氧化硅基空心球，中空微球的含量为5～20wt％，其烧成温度为500～900℃，粒径为10～60μm；
(2)在步骤(1)所得浆料中加入表面活性剂对陶瓷粉体进行疏水化修饰，所述表面活性剂为十二烷基硫酸钠和/或十六烷基硫酸钠，其加入量为总浆料质量的0.03～0.3wt％；
(3)通过机械搅拌方式对步骤(2)所得浆料进行发泡，得到陶瓷颗粒和中空微球协同稳定的泡沫；
(4)将步骤(3)所得泡沫干燥后进行烧结，获得具有连通孔壁的泡沫陶瓷，泡沫材料具有40～200μm的一级宏孔结构，孔壁由空心球堆积紧密而成，孔壁具有均匀的开孔结构，开孔孔径大小为10～60μm。
2.根据权利要求1所述的泡沫陶瓷，其特征在于：步骤(1)中所述陶瓷粉体为氧化铝、氧化铈、氧化锆或莫来石，其粒径范围为0.2～4.5μm。
3.根据权利要求1所述的泡沫陶瓷，其特征在于：步骤(3)中所获得的泡沫具有稳定性，中空微球均匀地分布在整个泡沫体系中。
4.根据权利要求1所述的泡沫陶瓷，其特征在于：步骤(4)中采用的烧结温度为1350～1600℃。
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| US20230136926A1 (en) * | 2020-04-07 | 2023-05-04 | Corning Incorporated | Porous structure such as for filters, and making the same |
| CN112028659B (zh) * | 2020-08-13 | 2021-09-10 | 湖南大学 | 一种碳石墨材料及其制备方法 |
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