CN107892577B - 一种Al4SiC4及Al4C3复合增强的碳化硅蜂窝陶瓷及其制备方法 - Google Patents

一种Al4SiC4及Al4C3复合增强的碳化硅蜂窝陶瓷及其制备方法 Download PDF

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CN107892577B
CN107892577B CN201711026625.5A CN201711026625A CN107892577B CN 107892577 B CN107892577 B CN 107892577B CN 201711026625 A CN201711026625 A CN 201711026625A CN 107892577 B CN107892577 B CN 107892577B
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honeycomb ceramic
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丁军
吴郑敏
邓承继
孔秋民
陈明祥
祝洪喜
余超
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NANJING KERUI SPECIAL CERAMICS CO Ltd
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Abstract

本申请公开了Al4SiC4及Al4C3复合增强的碳化硅蜂窝陶瓷的制备方法：以碳化硅粉A、碳化硅粉B、Al4SiC4和Al4C3粉为主料，外加主料2～10wt％的金属氧化物作为烧结助剂，以主料的质量为基准，将9wt％的纤维素，2～4wt％的表面活性剂，1～3wt％的植物油及2～5wt％的甘油溶于等质量的水后作为结合剂，将主料、烧结助剂及结合剂等混合均匀，得到混合料；将混合料倒入真空挤出机中成型，烘干，得到蜂窝陶瓷坯体；将蜂窝陶瓷坯体在氩气气氛条件下，升温至1900～2200℃，保温2～4h；自然冷却，即得。本申请还公开了采用上述方法制备的Al4SiC4及Al4C3复合增强的碳化硅蜂窝陶瓷。本发明原料利用率高，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，微观结构良好，微孔分布均匀，机械强度高。

Description

一种Al4SiC4及Al4C3复合增强的碳化硅蜂窝陶瓷及其制备方法
技术领域
本发明属于蜂窝陶瓷技术领域。具体涉及Al4SiC4及Al4C3复合增强的碳化硅蜂窝陶瓷及其制备方法。
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，主要采用壁流式蜂窝陶瓷过滤器。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主要有添加烧结助剂、挤出成型组合技术及压力注浆成型技术等。这些方法得到的壁流式碳化硅蜂窝陶瓷的抗热震性、抗热疲劳性能及工作的可靠性差，烧成温度高，壁内微孔大小及分布不均匀，产品性能较差，使用寿命短，生产成本高。
发明内容
本发明旨在克服现有技术缺陷，目的是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及Al4C3复合增强的碳化硅蜂窝陶瓷制备方法，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。
为实现上述目的，本发明所采用的技术方案的具体步骤是：
步骤一、将主料、烧结助剂和结合剂混合均匀，得到混合料；
所述主料包括25～35wt％的碳化硅粉A、55～65wt％的碳化硅粉B、1～5wt％的Al4SiC4和 1～5wt％的Al4C3粉；
所述烧结助剂为金属氧化物，以主料的质量为基准，烧结助剂的用量为2～10wt％；
所述结合剂为将纤维素和表面活性剂、植物油及甘油溶入等质量的水并搅拌均匀后所得，以主料的质量为基准，9wt％的纤维素，2～4wt％的表面活性剂，1～3wt％的植物油及2～5wt％的甘油；
步骤二、将所述混合料倒入真空挤出机中成型，在70～120℃条件下干燥6～14h，得到蜂窝陶瓷坯体；
步骤三、将所述蜂窝陶瓷坯体放入真空热压炉中，在氩气气氛条件下，以3～7℃/min升温至1900～2200℃，保温2～4h；自然冷却，即得Al4SiC4及Al4C3复合增强的碳化硅蜂窝陶瓷。
所述碳化硅粉A的纯度为85～99.9wt％；粒度为5～50μm。
所述碳化硅粉B的纯度为85～99.9wt％；粒度为0.05～0.5μm。
所述Al4SiC4的纯度为95～99.5wt％；粒度为30～80μm。
所述Al4C3粉的纯度为90～99wt％；粒度为10～100μm。
所述金属氧化物是氧化铝和氧化铁中的至少一种；纯度为≥98wt％。
所述纤维素是羟甲基纤维素、羟乙基纤维素与羟甲基纤维素钠中的至少一种。
所述表面活性剂是木质素磺酸盐、重烷基苯磺酸盐与烷基磺酸盐中的至少一种。
所述植物油是八角油、山苍子油与乌桕油中的至少一种。
由于采用上述技术方案，本发明与现有技术相比具有如下积极效果：
本发明以两种规格的碳化硅粉、Al4SiC4及Al4C3粉为主料，各种主料在市场上具有大量的供货，成本低廉，Al4SiC4主料为自制，掌握核心制备方法；其制备工艺是在主料中加入烧结助剂和结合剂，然后经混合、挤压成型，再经干燥，高温烧结而成，整个工艺流程的步骤紧凑，制品易于成型，且过程易于控制。
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，向碳化硅蜂窝陶瓷中引入Al4SiC4及Al4C3粉后，高温下Al4SiC4及Al4C3粉中铝元素固溶到碳化硅晶粒中，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15.0～ 21.0MPa。
因此，本发明具有原料利用率高，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，制品易成型和过程易于控制的特点，用该方法制备的Al4SiC4及Al4C3复合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。
本申请还提供了一种Al4SiC4及Al4C3复合增强的碳化硅蜂窝陶瓷，其采用上述的Al4SiC4及Al4C3复合增强的碳化硅蜂窝陶瓷的制备方法所制备。
该Al4SiC4及Al4C3复合增强的碳化硅蜂窝陶瓷的微孔大小均一，分布均匀，耐压强度为 15.0～21.0MPa。
附图说明
图1为本发明制备的一种Al4SiC4及Al4C3复合增强的碳化硅蜂窝陶瓷的正面孔结构图；
图2为图1所示Al4SiC4及Al4C3复合增强的碳化硅蜂窝陶瓷SEM图。
具体实施方案
下面结合附图和具体实施方式对本发明作进一步描述，并非对其保护范围的限制。实施方案中所需原料及试剂均市售可得。
为避免重复，先将本具体实施方式的原料描述如下，实施例中不再赘述：
所述碳化硅粉A的纯度为85～99.9wt％；粒度为5～50μm。
所述碳化硅粉B的纯度为85～99.9wt％；粒度为0.05～0.5μm。
所述Al4SiC4的纯度为95～99.5wt％；粒度为30～80μm。
所述Al4C3粉的纯度为90～99wt％；粒度为10～100μm。
所述金属氧化物是氧化铝和氧化铁中的至少一种；纯度为≥98wt％。
所述纤维素是羟甲基纤维素、羟乙基纤维素与羟甲基纤维素钠中的至少一种。
所述表面活性剂是木质素磺酸盐、重烷基苯磺酸盐与烷基磺酸盐中的至少一种。
所述植物油是八角油、山苍子油与乌桕油中的至少一种。
实施例1
一种Al4SiC4及Al4C3复合增强的碳化硅蜂窝陶瓷及其制备方法。本实施例所述制备方法的步骤是：
步骤一、将主料、烧结助剂和结合剂混合均匀，得到混合料；
所述主料包括35wt％的碳化硅粉A、55wt％的碳化硅粉B、5wt％的Al4SiC4和5wt％的 Al4C3粉；
所述烧结助剂为金属氧化物，以主料的质量为基准，烧结助剂的用量为4wt％；
所述结合剂为将纤维素和表面活性剂、植物油及甘油溶入等质量的水并搅拌均匀后所得，以主料的质量为基准，9wt％的纤维素，2wt％的表面活性剂，1wt％的植物油及2wt％的甘油；
步骤二、将所述混合料倒入真空挤出机中成型，在70℃条件下干燥6h，得到蜂窝陶瓷坯体；
步骤三、将所述蜂窝陶瓷坯体放入真空热压炉中，在氩气气氛条件下，以3℃/min升温至1900℃，保温2h；自然冷却，即得Al4SiC4及Al4C3复合增强的碳化硅蜂窝陶瓷。
在本实施例中，金属氧化物采用氧化铝，纤维素是羟甲基纤维素，表面活性剂是烷基磺酸盐，植物油是乌桕油。
本实施例制备的Al4SiC4及Al4C3复合增强的碳化硅蜂窝陶瓷经检测：中位孔径为4～16μm；耐压强度为15.8～17.2MPa。
实施例2
一种Al4SiC4及Al4C3复合增强的碳化硅蜂窝陶瓷及其制备方法。本实施例所述制备方法的步骤是：
步骤一、将主料、烧结助剂和结合剂混合均匀，得到混合料；
所述主料包括25wt％的碳化硅粉A、65wt％的碳化硅粉B、5wt％的Al4SiC4和5wt％的 Al4C3粉；
所述烧结助剂为金属氧化物，以主料的质量为基准，烧结助剂的用量为6wt％；
所述结合剂为将纤维素和表面活性剂、植物油及甘油溶入等质量的水并搅拌均匀后所得，以主料的质量为基准，9wt％的纤维素，3wt％的表面活性剂，2wt％的植物油及3wt％的甘油；
步骤二、将所述混合料倒入真空挤出机中成型，在80℃条件下干燥8h，得到蜂窝陶瓷坯体；
步骤三、将所述蜂窝陶瓷坯体放入真空热压炉中，在氩气气氛条件下，以5℃/min升温至2000℃，保温3h；自然冷却，即得Al4SiC4及Al4C3复合增强的碳化硅蜂窝陶瓷。
在本实施例中，金属氧化物采用氧化铁，纤维素是羟甲基纤维素，表面活性剂是木质素磺酸盐，植物油是八角油。
本实施例制备的Al4SiC4及Al4C3复合增强的碳化硅蜂窝陶瓷经检测：中位孔径为4～8μm；耐压强度为17.3～19.6MPa。
实施例3
一种Al4SiC4及Al4C3复合增强的碳化硅蜂窝陶瓷及其制备方法。本实施例所述制备方法的步骤是：
步骤一、将主料、烧结助剂和结合剂混合均匀，得到混合料；
所述主料包括30wt％的碳化硅粉A、62wt％的碳化硅粉B、4wt％的Al4SiC4和4wt％的 Al4C3粉；
所述烧结助剂为金属氧化物，以主料的质量为基准，烧结助剂的用量为7wt％；
所述结合剂为将纤维素和表面活性剂、植物油及甘油溶入等质量的水并搅拌均匀后所得，以主料的质量为基准，9wt％的纤维素，4wt％的表面活性剂，1wt％的植物油及2wt％的甘油；
步骤二、将所述混合料倒入真空挤出机中成型，在100℃条件下干燥6～14h，得到蜂窝陶瓷坯体；
步骤三、将所述蜂窝陶瓷坯体放入真空热压炉中，在氩气气氛条件下，以5℃/min升温至2100℃，保温2h；自然冷却，即得Al4SiC4及Al4C3复合增强的碳化硅蜂窝陶瓷。
在本实施例中，金属氧化物采用氧化铝，纤维素是羟甲基纤维素钠，表面活性剂是重烷基苯磺酸盐，植物油是山苍子油。
本实施例制备的Al4SiC4及Al4C3复合增强的碳化硅蜂窝陶瓷经检测：中位孔径为6～12μm；耐压强度为16.3～19.6MPa。
实施例4
一种Al4SiC4及Al4C3复合增强的碳化硅蜂窝陶瓷及其制备方法。本实施例所述制备方法的步骤是：
步骤一、将主料、烧结助剂和结合剂混合均匀，得到混合料；
所述主料包括34wt％的碳化硅粉A、64wt％的碳化硅粉B、1wt％的Al4SiC4和1wt％的 Al4C3粉；
所述烧结助剂为金属氧化物，以主料的质量为基准，烧结助剂的用量为8wt％；
所述结合剂为将纤维素和表面活性剂、植物油及甘油溶入等质量的水并搅拌均匀后所得，以主料的质量为基准，9wt％的纤维素，2.5wt％的表面活性剂，2.5wt％的植物油及2.5wt％的甘油；
步骤二、将所述混合料倒入真空挤出机中成型，在110℃条件下干燥10h，得到蜂窝陶瓷坯体；
步骤三、将所述蜂窝陶瓷坯体放入真空热压炉中，在氩气气氛条件下，以4℃/min升温至2200℃，保温2h；自然冷却，即得Al4SiC4及Al4C3复合增强的碳化硅蜂窝陶瓷。
在本实施例中，金属氧化物采用氧化铝和氧化铁的混合物，纤维素是羟乙基纤维素与羟甲基纤维素钠的混合物，表面活性剂是重烷基苯磺酸盐与烷基磺酸盐的混合物，植物油是山苍子油与乌桕油的混合物。
本实施例制备的Al4SiC4及Al4C3复合增强的碳化硅蜂窝陶瓷经检测：中位孔径为8～14μm；耐压强度为15.3～18.6MPa。

Claims (10)

1.一种Al4SiC4及Al4C3复合增强的碳化硅蜂窝陶瓷的制备方法，其特征在于所述制备方法的步骤：
将主料、烧结助剂和结合剂混合均匀，得到混合料；
所述主料包括25～35wt％的碳化硅粉A、55～65wt％的碳化硅粉B、1～5wt％的Al4SiC4和1～5wt％的Al4C3粉；
所述烧结助剂为金属氧化物，以主料的质量为基准，烧结助剂的用量为2～10wt％；
所述结合剂为将纤维素和表面活性剂、植物油及甘油溶入等质量的水并搅拌均匀后所得，以主料的质量为基准，9wt％的纤维素，2～4wt％的表面活性剂，1～3wt％的植物油及2～5wt％的甘油；
步骤二、将所述混合料倒入真空挤出机中成型，在70～120℃条件下干燥6～14h，得到蜂窝陶瓷坯体；
步骤三、将所述蜂窝陶瓷坯体放入真空热压炉中，在氩气气氛条件下，以3～7℃/min升温至1900～2200℃，保温2～4h；自然冷却，即得Al4SiC4及Al4C3复合增强的碳化硅蜂窝陶瓷。
2.根据权利要求1所述Al4SiC4及Al4C3复合增强的碳化硅蜂窝陶瓷的制备方法，其特征在于所述碳化硅粉A的纯度为85～99.9wt％；碳化硅粉A粒度为5～50μm。
3.根据权利要求1所述Al4SiC4及Al4C3复合增强的碳化硅蜂窝陶瓷的制备方法，其特征在于所述碳化硅粉B的纯度为85～99.9wt％；碳化硅粉B粒度为0.05～0.5μm。
4.根据权利要求1所述Al4SiC4及Al4C3复合增强的碳化硅蜂窝陶瓷的制备方法，其特征在于所述Al4SiC4的纯度为95～99.5wt％；粒度为30～80μm。
5.根据权利要求1所述Al4SiC4及Al4C3复合增强的碳化硅蜂窝陶瓷的制备方法，其特征在于所述Al4C3粉的纯度为90～99wt％；粒度为10～100μm。
6.根据权利要求1所述Al4SiC4及Al4C3复合增强的碳化硅蜂窝陶瓷的制备方法，其特征在于所述金属氧化物是氧化铝和氧化铁中的至少一种；纯度为≥98wt％。
7.根据权利要求1所述Al4SiC4及Al4C3复合增强的碳化硅蜂窝陶瓷的制备方法，其特征在于所述纤维素是羟甲基纤维素、羟乙基纤维素与羟甲基纤维素钠中的至少一种。
8.根据权利要求1所述Al4SiC4及Al4C3复合增强的碳化硅蜂窝陶瓷的制备方法，其特征在于所述表面活性剂是木质素磺酸盐、重烷基苯磺酸盐与烷基磺酸盐中的至少一种。
9.根据权利要求1所述Al4SiC4及Al4C3复合增强的碳化硅蜂窝陶瓷的制备方法，其特征在于所述植物油是八角油、山苍子油与乌桕油中的至少一种。
10.Al4SiC4及Al4C3复合增强的碳化硅蜂窝陶瓷，其特征在于所述Al4SiC4及Al4C3复合增强的碳化硅蜂窝陶瓷是根据权利要求1～9项中任一项所述Al4SiC4及Al4C3复合增强的碳化硅蜂窝陶瓷的制备方法所制备的Al4SiC4及Al4C3复合增强的碳化硅蜂窝陶瓷。
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