CN106565226B - 一种具有三维网络结构的硅酸铝多孔陶瓷材料的流延成型制备方法 - Google Patents

一种具有三维网络结构的硅酸铝多孔陶瓷材料的流延成型制备方法 Download PDF

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CN106565226B
CN106565226B CN201610872490.3A CN201610872490A CN106565226B CN 106565226 B CN106565226 B CN 106565226B CN 201610872490 A CN201610872490 A CN 201610872490A CN 106565226 B CN106565226 B CN 106565226B
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alumina silicate
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green compact
polycrystalline fibre
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徐泽跃
彭文博
陆丽芳
伦文山
许小静
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JIANGSU PROV CERAMIC RESEARCH INST Co Ltd
Jiangsu Jiuwu Hi Tech Co Ltd
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Abstract

本发明公开了一种具有三维网络结构的硅酸铝多孔陶瓷材料的流延成型制备方法。其步骤如下：将硅酸铝多晶纤维、硅酸铝陶瓷细粉、粘结剂、增塑剂、分散剂加入到水中，混合均匀并通过真空搅拌消泡得到稳定的浆料，将制成的浆料在流延机上成型得到硅酸铝多晶纤维薄膜生坯，然后将薄膜生坯层叠，经过干燥、排胶、烧结，得到晶粒与纤维相互连结而成具有三维网络结构的多孔陶瓷材料。该材料具有晶体和纤维相互连接所形成的网络结构，在具有高的孔隙率和过滤通量的同时具有优异的机械强度。

Description

一种具有三维网络结构的硅酸铝多孔陶瓷材料的流延成型制 备方法
技术领域
本发明涉及一种具有三维网络结构的硅酸铝多孔陶瓷材料的流延成型制备方法，属于陶瓷材料技术领域。
背景技术
流延法在陶瓷领域的应用主要是用来成型薄膜状的产品，该工艺具有设备工艺简单、颗连续化生产、生产效率高、产品性能优异和技术相对成熟的优势。本发明将流延法应用于生产具有三维网络结构的多孔陶瓷材料，不仅能够实现对材料显微结构的控制，而且所得到的材料在高孔隙率的同时保持较高的机械强度。流延成型又分为有机流延成型和水基流延成型，本发明采用的是水基流延成型，降低了成本，减小了对环境的危害。
传统的固液分离和固气分离陶瓷膜主要有两种类型，第一种是以陶瓷细粉为主要原料，通过成型和烧成得到所需的多孔陶瓷材料，孔隙源于颗粒堆积时形成的颗粒间的缝隙。目前主要有碳化硅、氮化硅、莫来石、堇青石等陶瓷粉体制成的多孔陶瓷膜，这些产品具有较好的力学性能，但孔隙率较低（一般≤40%），流体通过时的阻力较高，不适合在低压力或高通量下的应用。第二种是用硅酸铝多晶纤维作为主要原料通过压制、编织以及抽滤等方法成型和烧成所得到的陶瓷膜，它们具有较高的孔隙率，流体通过时的阻力较低，适合在低压力或高通量下的应用。但同时这类材料的力学性能较低，在使用时需要额外支撑或因为抗冲刷性能不佳，使用寿命短，其应用也受到很大的限制。
发明内容
本发明针对现有技术的不足，提供了一种具有三维网络结构的硅酸铝多孔陶瓷材料的流延成型制备方法，其采用流延成型制备纤维薄膜，可以使纤维在流延时能顺沿平面方向进行延展，实现排列有序，同时硅酸铝陶瓷颗粒稳定均匀分散在流延浆料中，也就实现在纤维结构中的均匀分布，能够实现纤维与颗粒的多点接触，这些颗粒和纤维间的接触点通过烧结形成相互间的连接，最终形成具有三维网络结构的多孔陶瓷材料。这种三维网络结构不仅使材料保持较高的孔隙率，而且能够使材料在高孔隙率时具备良好的机械强度和抗冲刷性能。
为实现本发明目的，提供了以下技术方案：．一种具有三维网络结构的硅酸铝多孔陶瓷材料的流延成型制备方法，其特征在于包含如下步骤：
（1）制备硅酸铝多晶纤维薄膜生坯：称取硅酸铝多晶纤维、硅酸铝陶瓷细粉、分散剂、粘结剂、增塑剂和水，置于容器中搅拌混合均匀成浆料，然后对浆料进行真空搅拌15~20min，以消除料浆中的气泡，将处理后的浆料在流延机上成型，得到厚度为0.8 ~ 2.0mm的硅酸铝多晶纤维薄膜生坯；
（2）制备中间层粘结料：称取短切硅酸铝多晶纤维、硅酸铝陶瓷细粉、分散剂、粘结剂和水，搅拌混合均匀后再真空搅拌10~20min；
（3）多层膜叠合：在硅酸铝多晶纤维薄膜生坯表面均匀涂覆中间层粘结料，涂覆厚度0.1~0.3mm，然后根据需要将涂覆粘结料的硅酸铝多晶纤维薄膜生坯叠合到所需要厚度，对叠合的硅酸铝多晶纤维薄膜生坯在厚度方向加压20-30MPa，保压2-3min得到多层膜；
（4）干燥：将多层膜放置于干燥烘箱内，在40℃下恒温干燥5~8h，再升温至80℃恒温干燥6~10h，干燥时间根据材料厚度调整；
（5）烧成：将烘干的多层膜置于氧化气氛窑炉中以0.3~1.2℃/min升温速度缓慢升温，在500℃-580℃保温2~3h排胶，在最高烧成温度1300~1400℃保温2~4h，随炉冷却到室温，得到具有三维网络结构的多孔陶瓷材料；
硅酸铝多晶纤维薄膜生坯以及中间层粘结料中的分散剂为聚丙烯酸铵，粘结剂为水玻璃、羧甲基纤维素钠、PVA、铝溶胶、硅溶胶中的一种或组合，增塑剂为邻苯二甲酸酯类。
硅酸铝多晶纤维薄膜生坯各组份以重量百分比计为：硅酸铝多晶纤维含量40.1~49.7wt%，硅酸铝陶瓷细粉8.3~15.4wt%，分散剂0.3~2.0wt%，粘结剂1.0~3.0wt%，增塑剂0.5~2.0wt%，去离子水30.8~48.8wt%。
中间层粘结料各组分以重量百分比计为：短切硅酸铝多晶纤维为33.0~39.7wt%，硅酸铝陶瓷细粉12.6~20.5wt %，分散剂0.2~1.0wt%，粘结剂1~3.0wt%，去离子水40.9~46.5wt%。
作为优选，硅酸铝多晶纤维纤维长度≥5.0mm。
作为优选，短切硅酸铝多晶纤维纤维长度≤1.0mm。
本发明有益效果：本发明采用流延成型制备纤维薄膜，可以使纤维在流延时能顺沿平面方向进行延展，实现排列有序，同时硅酸铝陶瓷颗粒稳定均匀分散在流延浆料中，也就实现在纤维结构中的均匀分布，能够实现纤维与颗粒的多点接触，这些颗粒和纤维间的接触点通过烧结形成相互间的连接，最终形成具有三维网络结构的多孔陶瓷材料。这种三维网络结构不仅使材料保持较高的孔隙率，而且能够使材料在高孔隙率时具备良好的机械强度和抗冲刷性能。
具体实施方式
实施例1：
（1）制备硅酸铝多晶纤维薄膜生坯：将去离子水48.8kg注入搅拌器，并开动搅拌，依次称取聚丙烯酸铵0.3kg、长度≥5.0mm的硅酸铝多晶纤维40.1kg、细度为325目的硅酸铝陶瓷细粉8.3kg、硅溶胶0.3kg、浓度为10%的PVA溶液0.7kg ，邻苯二甲酸二乙酯0.5kg，按相隔1min时间依次加入搅拌器，搅拌30min后，再进行真空搅拌15min，得到所需浆料。将处理后的成型浆料在流延设备上以1.5cm/s 的速度流延，得到的湿膜在空气中干燥6h，得到厚度为0.8mm的硅酸铝多晶纤维薄膜生坯。
（2）制备中间层粘结料：将去离子水46.5kg注入搅拌器，并开动搅拌，依次称取聚丙烯酸铵0.2kg、长度≤1.0mm的短切硅酸铝多晶纤维39.7kg、细度为325目的硅酸铝陶瓷细粉12.6kg、硅溶胶0.5kg、浓度为10%的PVA溶液0.5kg，按相隔1min时间依次加入搅拌器，搅拌30min后，再进行真空搅拌15min，得到所需浆料。
（3）多层膜叠合：在步骤（1）所制硅酸铝多晶纤维薄膜生坯表面均匀涂覆步骤（2）所制中间层粘结料，涂覆厚度0.1mm，然后将10层涂覆粘结料的生坯膜按要求叠合，对叠合的生坯在厚度方向加压20MPa，保压3min。
（4）干燥：将步骤（3）所得材料放在烘箱内，40℃下恒温干燥5h，再升温至80℃干燥6h。
（5）烧成：将步骤（4）烘干的坯体置于窑炉中以1.2℃/min缓慢升温，其中在500℃保温3.0h排胶，在最高烧成温度1300℃保温4h，然后冷却到室温，得到具有三维网络结构的多孔陶瓷材料。
该多孔陶瓷材料孔隙率（阿基米德法）为71.3%，抗折强度（三点法）为7.2MPa。
实施例2：
（1）制备硅酸铝多晶纤维薄膜生坯：将去离子水35.3kg注入搅拌器，并开动搅拌，依次称取聚丙烯酸铵2.0kg、长度≥5.0mm的硅酸铝多晶纤维45.4kg、细度为325目的硅酸铝陶瓷细粉12.3kg、铝溶胶1.5kg、浓度为10%的PVA溶液1.5kg、邻苯二甲酸二乙酯2kg，按相隔1min时间依次加入搅拌器，搅拌30min后，再进行真空搅拌20min，得到所需浆料。将处理后的成型浆料在流延设备上以1.5cm/s 的速度流延，得到的湿膜在空气中干燥12h，得到厚度为1.3mm的硅酸铝多晶纤维薄膜生坯。
（2）制备中间层粘结料：将去离子水43.2kg注入搅拌器，并开动搅拌，依次称取聚丙烯酸铵0.6kg、长度≤1.0mm的短切硅酸铝多晶纤维36.0kg、细度为325目的硅酸铝陶瓷细粉17.2kg、铝溶胶1.5kg、浓度为10%的PVA溶液1.5kg、邻苯二甲酸酯1.4kg，按相隔1min时间依次加入搅拌器，搅拌30min后，再进行真空搅拌10min，得到所需浆料。
（3）多层膜叠合：在步骤（1）所制硅酸铝多晶纤维薄膜生坯表面均匀涂覆步骤（2）所制中间层粘结料，涂覆厚度0.20mm，然后将8层涂覆粘结料的生坯膜按要求叠合，对叠合的生坯在厚度方向加压20MPa，保压2min。
（4）干燥：将步骤（3）所得材料放在烘箱内，40℃下恒温干燥6h，再升温至80℃干燥8h。
（5）烧成：将步骤（4）烘干的坯体置于窑炉中以0.6℃/min缓慢升温，其中在520℃保温2h排胶，在最高烧成温度1400℃保温2h，然后冷却到室温，得到具有三维网络结构的多孔陶瓷材料。
所得到的多孔陶瓷材料孔隙率（阿基米德法）为60.1% ，抗折强度（三点法）为10.7MPa。
实施例3：
（1）制备硅酸铝多晶纤维薄膜生坯：将去离子水30.8kg注入搅拌器，并开动搅拌，依次称取长度≥5.0mm的硅酸铝多晶纤维49.7kg、细度为325目的硅酸铝陶瓷细粉15.4kg、聚丙烯酸铵0.8kg、铝溶胶0.8kg、浓度为10%的PVA溶液1.5kg ，邻苯二甲酸二乙酯1.0kg，按相隔1min时间依次加入搅拌器，搅拌30min后，再进行真空搅拌20min，得到所需浆料。将处理后的成型浆料在流延设备上以1.5cm/s 的速度流延，得到的湿膜在空气中干燥24h，得到厚度为2.0mm的硅酸铝多晶纤维薄膜生坯。
（2）制备中间层粘结料：将去离子水40.9 kg注入搅拌器，并开动搅拌，依次称取聚丙烯酸铵1.0kg、长度≤1.0mm的短切硅酸铝多晶纤维35.0kg、细度为325目的硅酸铝陶瓷细粉20.5kg、铝溶胶1.1kg、浓度为10%的PVA溶液1.5kg、邻苯二甲酸酯1.2kg，按相隔1min时间依次加入搅拌器，搅拌30min后，再进行真空搅拌20min，得到所需浆料。
（3）多层膜叠合：在步骤（1）所制硅酸铝多晶纤维薄膜生坯表面均匀涂覆步骤（2）所制中间层粘结料，涂覆厚度0.3mm，然后将6层涂覆粘结料的生坯膜按要求叠合，对叠合的生坯在厚度方向加压30MPa，保压2min。
（4）干燥：将步骤（3）所得材料放在烘箱内，40℃下恒温干燥8h，再升温至80℃干燥10h。
（5）烧成：将步骤（4）烘干的坯体置于窑炉中以0.3℃/min缓慢升温，在580℃保温2h排胶，在最高烧成温度1360℃保温2h，然后冷却到室温，得到具有三维网络结构的多孔陶瓷材料。
该多孔陶瓷材料孔隙率（阿基米德法）为55.3%，抗折强度（三点法）为12.7MPa。

Claims (1)

1.一种具有三维网络结构的硅酸铝多孔陶瓷材料的流延成型制备方法，其特征在于包含如下步骤：
（1）制备硅酸铝多晶纤维薄膜生坯：称取纤维长度≥5.0mm的硅酸铝多晶纤维40.1~49.7wt%、硅酸铝陶瓷细粉8.3~15.4wt%、分散剂0.3~2.0wt%、粘结剂1.0~3.0wt%、增塑剂0.5~2.0wt%和去离子水30.8~48.8wt%，置于容器中搅拌混合均匀成浆料，然后对浆料进行真空搅拌15~20min，以消除料浆中的气泡，将处理后的浆料在流延机上成型，得到厚度为0.8 ~2.0mm的硅酸铝多晶纤维薄膜生坯；
（2）制备中间层粘结料：称取纤维长度≤1.0mm的短切硅酸铝多晶纤维33.0~39.7wt%、硅酸铝陶瓷细粉12.6~20.5wt %、分散剂0.2~1.0wt%、粘结剂1~3.0wt%和去离子水40.9~46.5wt%，搅拌混合均匀后再真空搅拌10~20min；
（3）多层膜叠合：在硅酸铝多晶纤维薄膜生坯表面均匀涂覆中间层粘结料，涂覆厚度0.1~0.3mm，然后根据需要将涂覆粘结料的硅酸铝多晶纤维薄膜生坯叠合到所需要厚度，对叠合的硅酸铝多晶纤维薄膜生坯在厚度方向加压20-30MPa，保压2-3min得到多层膜；
（4）干燥：将多层膜放置于干燥烘箱内，在40℃下恒温干燥5~8h，再升温至80℃恒温干燥6~10h，干燥时间根据材料厚度调整；
（5）烧成：将烘干的多层膜置于氧化气氛窑炉中以0.3~1.2℃/min升温速度缓慢升温，在500℃-580℃保温2~3h排胶，在最高烧成温度1300~1400℃保温2~4h，随炉冷却到室温，得到具有三维网络结构的多孔陶瓷材料；
硅酸铝多晶纤维薄膜生坯以及中间层粘结料中的分散剂为聚丙烯酸铵，粘结剂为水玻璃、羧甲基纤维素钠、PVA、铝溶胶、硅溶胶中的一种或组合，增塑剂为邻苯二甲酸酯类。
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