CN113121258B - 一种高强度高孔隙率的多孔陶瓷及其制备方法 - Google Patents

一种高强度高孔隙率的多孔陶瓷及其制备方法 Download PDF

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CN113121258B
CN113121258B CN202110284412.2A CN202110284412A CN113121258B CN 113121258 B CN113121258 B CN 113121258B CN 202110284412 A CN202110284412 A CN 202110284412A CN 113121258 B CN113121258 B CN 113121258B
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殷波
郑益锋
廖佳
宋晓春
范昌龙
毛旭敏
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Yixing Morgan Thermal Ceramics Co ltd
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Abstract

本发明涉及一种高强度高孔隙率的多孔陶瓷及其制备方法，包括以下步骤：将2‑10wt%的聚醚多元醇、0.2‑2wt%的二甲基硅油和5‑30wt%的二甲苯混合、搅拌；加入50‑80wt%的氧化铝粉体，搅拌；加入2‑8wt%的二苯甲烷二异氰酸酯，搅拌；加入总量为0.2‑1wt%的三乙烯二胺和二月桂酸二丁基锡催化剂，搅拌；将固化后的陶瓷坯体放入80℃的烘箱中熟化12h，在高温电阻炉中以适宜的速率升温到1500‑1600℃并保温1‑2h，然后样品随炉冷却至室温后取出，制得高强度高孔隙率的多孔陶瓷。本发明通过优化氧化铝含量、有机物配方、催化剂配比及制备工艺等方法，制备的多孔陶瓷强度高、孔隙率高，具有成本低廉、工艺简单、易于工业化生产的特点。

Description

一种高强度高孔隙率的多孔陶瓷及其制备方法
技术领域
本发明属于多孔陶瓷技术领域，具体涉及一种高强度高孔隙率的多孔陶瓷及其制备方法。
背景技术
多孔陶瓷具有体积密度小、耐腐蚀性强、比表面积大等优点，被广泛应用于过滤分离、催化剂载体、保温隔热材料、生物材料等诸多领域，是一种重要的工业陶瓷材料。
有机泡沫浸渍法是制备多孔陶瓷的一种主要方法，它是以聚氨酯等有机泡沫模板浸渍陶瓷浆料，经干燥、排胶、烧成后得到具有高孔隙率和开孔结构的多孔陶瓷。虽然上述方法用来制备同时具有一定强度和孔隙率的多孔陶瓷具有一定的可行性，但在此工艺中，由于陶瓷浆料很难均匀地涂覆在有机泡沫骨架上，在烧成过程中易于产生空心支柱结构和开裂现象，导致材料的力学性能下降。因此，现有技术未获得同时具有高强度和高孔隙率（>80%）的多孔陶瓷。
鉴于上述技术缺陷，本发明公开了一种高强度高孔隙率的多孔陶瓷及其制备方法，制备获得了高孔隙率的氧化铝孔陶瓷并减少了陶瓷烧成体变形问题。
发明内容
本发明的目的是针对现有技术中难以制备兼具高强度和高孔隙率的多孔陶瓷的问题，提供了一种高强度高孔隙率的多孔陶瓷及其制备方法，通过优化氧化铝含量、有机物配方、催化剂配比及制备工艺等方法，获得了高强度高孔隙率的氧化铝多孔陶瓷。
为实现上述目的，本发明采用的技术方案是：
第一步，将聚醚多元醇、二甲基硅油、二甲苯加入到烧杯中，用电动搅拌机搅拌5min，搅拌速度为300r/min；
第二步，分批加入氧化铝粉体，搅拌5min，搅拌速度为400 r/min；
第三步，加入二苯甲烷二异氰酸酯，搅拌1min，搅拌速度为500r/min；
第四步，加入三乙烯二胺和二月桂酸二丁基锡催化剂，迅速搅拌10-15s，搅拌速度为700r/min；
第五步，将固化后的陶瓷坯体放入80℃的烘箱中熟化12h，在高温电阻炉中以适宜的速率升温到合适温度并保温烧成，样品随炉冷却至室温后取出，获得高强度高孔隙率的多孔陶瓷。
优选的，所述聚醚多元醇添加量为2-10wt%、二甲基硅油添加量为0.2-2wt%、二甲苯添加量为5-30wt%；
优选的，所述氧化铝粉体添加量为50-80wt%；
优选的，所述二苯甲烷二异氰酸酯添加量为2-8wt%；
优选的，所述三乙烯二胺和二月桂酸二丁基锡催化剂添加总量为0.2-1wt%，并且三乙烯二胺与二月桂酸二丁基锡质量比为1:2；
优选的，所述烧成温度为1500-1600℃，保温时间为1-2h。
与现有技术相比，本发明的有益效果是：
(1)本发明采用的原料易得，并通过优化氧化铝含量、有机物配方、催化剂配比及制备工艺等方法获得了高强度高孔隙率的氧化铝多孔陶瓷，成本低、工艺简单。
(2)图1是由不同方法制备的氧化铝多孔陶瓷的抗弯强度和孔隙率的关系。由图可见，在其他条件相同的情况下，当孔隙率为80%时，传统模板法制备的多孔陶瓷具有约为5MPa的抗弯强度，由本发明制备的多孔陶瓷约为11.5MPa抗弯强度。因此，本发明在不影响材料的高孔隙率性质的条件下，改善了模板法在强度上的不足，有效地弥补了多孔材料应用的局限性。并且，本发明易于加工处理制备复杂形状的多孔陶瓷构件。
附图说明
图1是本发明与传统模板法制备的多孔陶瓷的抗弯强度和孔隙率的对比图。
图2是本发明实施例1中制备的多孔陶瓷SEM图。
图3是本发明实施例2中制备的多孔陶瓷SEM图。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白，以下结合实施例，对本发明进行进一步详细说明；应当理解，此处所描述的具体实施例仅用以解释本发明，并不用于限定本发明；除非特别说明，本发明采用的原料、试剂、方法和设备为本技术领域常规试剂、方法和设备。
实施例1
本实施例提供一种高强度高孔隙率的多孔陶瓷及其制备方法：
第一步，将7wt%的聚醚多元醇、1wt%的二甲基硅油、25wt%二甲苯加入到烧杯中，用电动搅拌机搅拌5min，搅拌速度为300r/min；
第二步，加入60wt%氧化铝粉体，搅拌5min，搅拌速度为400 r/min；
第三步，加入6wt%的二苯甲烷二异氰酸酯，搅拌1min，搅拌速度为500r/min；
第四步，加入总量为1wt%为三乙烯二胺和二月桂酸二丁基锡催化剂，三乙烯二胺与二月桂酸二丁基锡质量比为1:2，迅速搅拌10-15s，搅拌速度为700r/min；
第五步，将固化后的陶瓷坯体放入80℃的烘箱中熟化12h，在高温电阻炉中以适宜的速率升温到1600℃，保温1h烧成，样品随炉冷却至室温后取出，获得高强度高孔隙率的多孔陶瓷。
对本实施例制备的多孔陶瓷进行SEM表征，结果如图2所示，多数孔隙保持了完整的球型结构，孔结构相对均匀，部分孔隙没有出现孔洞，这种闭孔结构和均匀的孔结构有利于减少泡沫陶瓷受力时的应力集中，并有助于提高材料的机械强度，降低导热系数。
此外，其他测试结果如下：氧化铝多孔陶瓷的孔隙率为80.2%，容重为0.72g/cm3，抗弯强度为12.8MPa。
以上结果表明，实施例1的制备方法，获得了高强度高孔隙率的多孔陶瓷。
实施例2
本实施例提供一种高强度高孔隙率的多孔陶瓷及其制备方法：
第一步，将10wt%的聚醚多元醇、1.5wt%的二甲基硅油、10wt%二甲苯加入到烧杯中，用电动搅拌机搅拌5min，搅拌速度为300r/min；
第二步，加入70wt%氧化铝粉体，搅拌5min，搅拌速度为400 r/min；
第三步，加入8wt%的二苯甲烷二异氰酸酯，搅拌1min，搅拌速度为500r/min；
第四步，加入总量为0.5wt%为三乙烯二胺和二月桂酸二丁基锡催化剂，三乙烯二胺与二月桂酸二丁基锡质量比为1:2，迅速搅拌10-15s，搅拌速度为700r/min；
第五步，将固化后的陶瓷坯体放入80℃的烘箱中熟化12h，在高温电阻炉中以适宜的速率升温到1550℃，保温2h烧成，样品随炉冷却至室温后取出，获得高强度高孔隙率的多孔陶瓷。
对本实施例制备的多孔陶瓷进行SEM表征，结果如图3所示，多数孔隙保持了完整的球型结构，孔结构相对均匀，该结果与图2类似。
此外，其他测试结果如下：氧化铝多孔陶瓷的孔隙率为82%，容重为0.7g/cm3，抗弯强度为10.3MPa。
以上结果表明，实施例2的制备方法，获得了高强度高孔隙率的多孔陶瓷。
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内，所做的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。

Claims (1)

1.一种高强度高孔隙率的多孔陶瓷的制备方法，其特征在于：
第一步，将聚醚多元醇、二甲基硅油、二甲苯加入到烧杯中，用电动搅拌机搅拌5min，搅拌速度为300r/min；
第二步，加入氧化铝粉体，搅拌5min，搅拌速度为400 r/min；
第三步，加入二苯甲烷二异氰酸酯，搅拌1min，搅拌速度为500r/min；
第四步，加入三乙烯二胺和二月桂酸二丁基锡催化剂，迅速搅拌10-15s，搅拌速度为700r/min；
第五步，将固化后的陶瓷坯体放入80℃的烘箱中熟化12h，在高温电阻炉中以适宜的速率升温到合适温度并保温烧成，样品随炉冷却至室温后取出，获得高强度高孔隙率的多孔陶瓷；
其中，所述聚醚多元醇添加量为2-10wt%、二甲基硅油添加量为0.2-2wt%、二甲苯添加量为5-30wt%；所述氧化铝粉体添加量为50-80wt%；所述二苯甲烷二异氰酸酯添加量为2-8wt%；所述三乙烯二胺和二月桂酸二丁基锡催化剂添加总量为0.2-1wt%，并且三乙烯二胺与二月桂酸二丁基锡质量比为1:2；所述烧成温度为1500-1600℃，保温时间为1-2h。
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