CN107814575B - 一种Al4SiC4增强的碳化硅蜂窝陶瓷及其制备方法 - Google Patents

一种Al4SiC4增强的碳化硅蜂窝陶瓷及其制备方法 Download PDF

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CN107814575B
CN107814575B CN201711073073.3A CN201711073073A CN107814575B CN 107814575 B CN107814575 B CN 107814575B CN 201711073073 A CN201711073073 A CN 201711073073A CN 107814575 B CN107814575 B CN 107814575B
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邓承继
吴郑敏
余超
孔秋民
陈明祥
祝洪喜
丁军
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JIANGSU GAOCHUN CERAMICS CO Ltd
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Abstract

本发明公开了一种Al4SiC4增强的碳化硅蜂窝陶瓷，原料组分包括：碳化硅粉一70~80份、碳化硅粉二10~20份、Al4SiC4 2~10份、烧结助剂5~15份、结合剂12.5‑15.5份和水12.5‑15.5份，所述份数为质量份数，其中，碳化硅粉一的纯度为85~99.9wt%，粒度为5~50μm；碳化硅粉二的纯度为85~99.9wt%，粒度为0.05~0.5μm。本发明Al4SiC4增强的碳化硅蜂窝陶瓷具有原料利用率高、生产效率高的特点，且制品结构为壁流式提高了对废气的净化能力，制品易成型和过程易于控制，Al4SiC4增强的碳化硅蜂窝陶瓷微观结构良好，微孔分布均匀，机械强度高，热膨胀系数低。

Description

一种Al4SiC4增强的碳化硅蜂窝陶瓷及其制备方法
技术领域
本发明涉及一种Al4SiC4增强的碳化硅蜂窝陶瓷及其制备方法，属于蜂窝陶瓷技术领域。
背景技术
发达国家于上世纪70年代开始机动车尾气治理，制定了排放标准。为降低汽柴油车尾气污染物的危害，主要采用蜂窝陶瓷过滤器。随着经济建设和居民生活用汽柴油车尾气排放量不断增加，我国对环保要求逐渐加大，需要更高的减排技术。
目前壁流式碳化硅蜂窝陶瓷的制备方法得到的壁流式碳化硅蜂窝陶瓷的热膨胀系数高，烧成温度高，壁内微孔大小及分布不均匀，产品机械性能较差，生产成本高。
发明内容
本发明提供一种原料利用率高，生产效率高，且制品结构为壁流式提高了对废气的净化能力的Al4SiC4增强的碳化硅蜂窝陶瓷及其制备方法，用该方法制备的碳化硅蜂窝陶瓷微观结构良好，微孔分布均匀，机械强度高。
为解决上述技术问题，本发明所采用的技术方案如下：
一种Al4SiC4增强的碳化硅蜂窝陶瓷，其原料组分包括：碳化硅粉一70～80份、碳化硅粉二10～20份、Al4SiC4 2～10份、烧结助剂5～15份、结合剂12.5-15.5份和水12.5-15.5份，所述份数为质量份数，其中，碳化硅粉一的纯度为85～99.9wt％，粒度为5～50μm；碳化硅粉二的纯度为85～99.9wt％，粒度为0.05～0.5μm。
由上述原料所制备的Al4SiC4增强的碳化硅蜂窝陶瓷抗热震性强、抗热疲劳性能强、工作的可靠性好，烧成温度低，壁内微孔大小及分布均匀，产品机械强度高，使用寿命长，生产成本低。
为了进一步提高碳化硅蜂窝陶瓷的结构强度，烧结助剂为金属氧化物。优选，金属氧化物为氧化铝或氧化钇中的至少一种。进一步优选，金属氧化物的纯度为≥98wt％。
为了进一步促进各组分之间的协同效应，提高碳化硅蜂窝陶瓷的抗热震性、抗热疲劳性能和结构强度，结合剂包括纤维素7～8份和添加剂5.5～7.5份，所述份数为质量份数，其中，添加剂为表面活性剂、甘油或植物油中的至少一种。优选，结合剂包括纤维素7.5份、表面活性剂1-3份、植物油3-6份和甘油2-4份，所述份数为质量份数。
为了进一步提高产品的力学性能和微孔均匀性，优选，纤维素为乙基纤维素、羟甲基纤维素或羧甲基纤维素钠中的至少一种；表面活性剂为脂肪醇聚氧乙烯醚硫酸钠、烷基聚醚或脂肪醇聚氧乙烯醚中的至少一种；植物油为松节油、樟树油或桉树油中的至少一种。
为了进一步提高碳化硅蜂窝陶瓷的结构强度，Al4SiC4的纯度为95～99.5wt％，粒度为 30～80μm。
上述Al4SiC4增强的碳化硅蜂窝陶瓷的制备方法，包括如下步骤：
步骤一、将碳化硅粉一、碳化硅粉二、Al4SiC4、烧结助剂、结合剂和水，混合均匀，得到混合料；
步骤二、将所述混合料倒入真空挤出机中成型，并在60～110℃条件下干燥12～24h，得到蜂窝陶瓷坯体；
步骤三、将蜂窝陶瓷坯体放入真空热压炉中，在氩气气氛条件下，以5～10℃/min升温至2000～2200℃，保温1～3h后，自然冷却，即得Al4SiC4增强的碳化硅蜂窝陶瓷。
上述制备方法原料利用率高，生产效率高，且制品结构为壁流式提高了对废气的净化能力，用该方法制备的碳化硅蜂窝陶瓷微观结构良好，微孔分布均匀，机械强度高。
本发明以碳化硅粉和Al4SiC4为原料，成本低廉；其制备工艺是在原料中加入结合剂，混合，挤压成型，干燥，高温烧成，即得壁流式碳化硅蜂窝陶瓷，制品易成型和过程易于控制。
本发明采用添加结合剂与挤压成型相结合的方式制备壁流式碳化硅蜂窝陶瓷坯体，再经高温烧成制得壁流式碳化硅蜂窝陶瓷。SiC由于是共价性极强的化合物，高温烧结困难。同时碳化硅陶瓷制备用原料的可塑性差，采用挤压成型工艺的成品率低。而壁流式碳化硅蜂窝陶瓷需要在薄壁上设置10微米左右的贯通微孔，微孔大小、数量及分布可控，其制备技术要求高。通过采用添加结合剂与挤压成型相结合的方式可提高原料的可塑性及产品的成品率，控制微孔大小、数量及分布。
另外，申请人经研究还发现，向碳化硅蜂窝陶瓷中引入Al4SiC4后，高温下Al4SiC4中铝元素固溶到碳化硅晶粒中，占据了碳化硅中的硅位点，形成堆叠结构，使碳化硅晶型生长为规则的六方晶型；随着碳化硅在高温下的分解、挥发与重结晶，其六方晶粒顶点互相连接共同生长，呈现良好的骨架结构；这种晶粒间互连共生的结合方式也使材料内部产生较多的微小孔隙，提升材料的透气性及吸附性能；添加的金属氧化物高温下形成液相，促使试样烧结更为致密，提高陶瓷的机械性能；热处理后得到的壁流式碳化硅蜂窝陶瓷微孔大小均一，分布均匀，耐压强度为13.0～18.0MPa。
本发明未提及的技术均参照现有技术。
本发明Al4SiC4增强的碳化硅蜂窝陶瓷具有原料利用率高、生产效率高的特点，且制品结构为壁流式提高了对废气的净化能力，制品易成型和过程易于控制，用该方法制备的Al4O4C增强的碳化硅蜂窝陶瓷微观结构良好，微孔分布均匀，机械强度高，热膨胀系数低。
附图说明
图1为本发明实施例1所得的Al4O4C增强的碳化硅蜂窝陶瓷的正面孔结构图；
图2为图1所示Al4O4C增强的碳化硅蜂窝陶瓷SEM图。
具体实施方式
为了更好地理解本发明，下面结合实施例进一步阐明本发明的内容，但本发明的内容不仅仅局限于下面的实施例。
下述各例中，Al4SiC4增强的碳化硅蜂窝陶瓷的原料组分包括：碳化硅粉一70～80份、碳化硅粉二10～20份、Al4SiC42～10份、烧结助剂5～15份、结合剂12.5-15.5份和水12.5-15.5 份，所述份数为质量份数，其中，碳化硅粉一的纯度为99wt％，粒度为5～50μm，厂家为安阳金晟冶金材料有限公司；碳化硅粉二的纯度为99wt％，粒度为0.05～0.5μm，厂家为安阳金晟冶金材料有限公司；Al4SiC4的纯度为99wt％，粒度为30～80μm。
烧结助剂为氧化铝或氧化钇中的至少一种；金属氧化物的纯度为99wt％。
结合剂包括纤维素7.5份、表面活性剂1-3份、植物油3-6份和甘油2-4份，所述份数为质量份数。
上述Al4SiC4增强的碳化硅蜂窝陶瓷的制备方法，包括如下步骤：
步骤一、将碳化硅粉一、碳化硅粉二、Al4SiC4、烧结助剂、结合剂和水，混合均匀，得到混合料；
步骤二、将所述混合料倒入真空挤出机中成型，并在60～110℃条件下干燥12～24h，得到蜂窝陶瓷坯体；
步骤三、将蜂窝陶瓷坯体放入真空热压炉中，在氩气气氛条件下，以5～10℃/min升温至2000～2200℃，保温1～3h后，自然冷却，即得Al4SiC4增强的碳化硅蜂窝陶瓷。
表1各实施例的原料组分表
Figure BDA0001457400900000041
表2各实施例制备的工艺条件
Figure BDA0001457400900000042
表2中干燥温度和干燥时间对应上述步骤二中的温度和时间；升温速率、温度和保温时间对应步骤三中的升温速率、温度和保温时间。
表3各实施例所用的烧结助剂和结合剂等
Figure BDA0001457400900000043
Figure BDA0001457400900000051
表3中，乙基纤维素，为分析纯，粘度10为500g，购自南京奥佳化工有限公司；羟甲基纤维素，密度0.0001g/cm3，购自上海中一化工有限公司；羧甲基纤维素钠，陶瓷级，购自河北绿能科技有限公司；烷基聚醚，为烷基环氧基聚醚，购自扬州晨化型材料股份有限公司；脂肪醇聚氧乙烯醚，为平平加O-20，购自扬州晨化型材料股份有限公司；脂肪醇聚氧乙烯醚硫酸钠，购自苏州源泰润化工有限公司。
表4各实施例所得产品的性能表
Figure BDA0001457400900000052

Claims (8)

1.一种Al4SiC4增强的碳化硅蜂窝陶瓷，其特征在于：其原料组分包括：碳化硅粉一70~80份、碳化硅粉二10~20份、Al4SiC4 2~10份、烧结助剂5~15份、结合剂12.5-15.5份和水12.5-15.5份，所述份数为质量份数，其中，碳化硅粉一的纯度为85~99.9wt%，粒度为5~50μm；碳化硅粉二的纯度为85~99.9wt%，粒度为0.05~0.5μm；
Al4SiC4的纯度为95~99.5wt%，粒度为30~80μm；
该Al4SiC4增强的碳化硅蜂窝陶瓷采用如下步骤制备：
步骤一、将碳化硅粉一、碳化硅粉二、Al4SiC4、烧结助剂、结合剂和水，混合均匀，得到混合料；
步骤二、将所述混合料倒入真空挤出机中成型，并在60~110℃条件下干燥12~24h，得到蜂窝陶瓷坯体；
步骤三、将蜂窝陶瓷坯体放入真空热压炉中，在氩气气氛条件下，以5~10℃/min升温至2000~2200℃，保温1~3h后，自然冷却，即得Al4SiC4增强的碳化硅蜂窝陶瓷。
2.如权利要求1所述的Al4SiC4增强的碳化硅蜂窝陶瓷，其特征在于：烧结助剂为金属氧化物。
3.如权利要求2所述的Al4SiC4增强的碳化硅蜂窝陶瓷，其特征在于：金属氧化物为氧化铝或氧化钇中的至少一种。
4.如权利要求2所述的Al4SiC4增强的碳化硅蜂窝陶瓷，其特征在于：金属氧化物的纯度为≥98wt%。
5.如权利要求1-4任意一项所述的Al4SiC4增强的碳化硅蜂窝陶瓷，其特征在于：结合剂包括纤维素7~8份和添加剂5.5~7.5份，所述份数为质量份数，其中，添加剂为表面活性剂、甘油或植物油中的至少一种。
6.如权利要求5所述的Al4SiC4增强的碳化硅蜂窝陶瓷，其特征在于：结合剂包括纤维素7.5份、表面活性剂1-3份、植物油3-6份和甘油2-4份，所述份数为质量份数。
7.如权利要求5所述的Al4SiC4增强的碳化硅蜂窝陶瓷，其特征在于：纤维素为乙基纤维素、羟甲基纤维素或羧甲基纤维素钠中的至少一种。
8.如权利要求5所述的Al4SiC4增强的碳化硅蜂窝陶瓷，其特征在于：表面活性剂为脂肪醇聚氧乙烯醚硫酸钠、烷基聚醚或脂肪醇聚氧乙烯醚中的至少一种；植物油为松节油、樟树油或桉树油中的至少一种。
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