CN109678517B - 一种原位AlN-B4C增强的碳化硅蜂窝陶瓷及其制备方法 - Google Patents

一种原位AlN-B4C增强的碳化硅蜂窝陶瓷及其制备方法 Download PDF

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CN109678517B
CN109678517B CN201910160682.5A CN201910160682A CN109678517B CN 109678517 B CN109678517 B CN 109678517B CN 201910160682 A CN201910160682 A CN 201910160682A CN 109678517 B CN109678517 B CN 109678517B
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silicon carbide
honeycomb ceramic
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邓承继
柯露
余超
丁军
祝洪喜
吴郑敏
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Wuhan University of Science and Engineering WUSE
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Abstract

本发明涉及一种原位AlN‑B4C增强的碳化硅蜂窝陶瓷及其制备方法。其技术方案是：先向主料中加入金属氧化物和结合剂，混合均匀；再将倒入真空挤出机中，成型，干燥；然后置入真空热压炉中，在氮气气氛中升温至1800～2200℃，保温，冷却，即得原位AlN‑B4C增强的碳化硅蜂窝陶瓷。所述主料是由65～75wt％的粒度为5～50μm的碳化硅粉、20～25wt％的粒度为0.05～0.5μm的碳化硅粉和3～11wt％的铝硼碳粉混合而成；所述金属氧化物的加入量为主料的1～5wt％；所述结合剂是由纤维素、表面活性剂、植物油、甘油和水混合而成。本发明生产效率高和生产成本低，所制制品微观结构良好、微孔分布均匀、机械强度高和对废气的净化能力强。

Description

一种原位AlN-B4C增强的碳化硅蜂窝陶瓷及其制备方法
技术领域
本发明属于碳化硅蜂窝陶瓷技术领域。具体涉及一种原位AlN-B4C增强的碳化硅蜂窝陶瓷及其制备方法。
背景技术
蜂窝陶瓷是由许多平行贯通的孔道组成的陶瓷，因其耐冲击和重量轻等特点，多作为汽车尾气催化剂载体。汽车尾气催化剂载体需要较高的抗热冲击性能和较高的机械强度，还需具备低的热容量、高的热导率才能使得催化剂在短时间内发挥作用。众所周知，汽车尾气催化剂载体的比表面积越大，可以负载的催化剂就越多，所以蜂窝陶瓷还要有较大的比表面积。此外，还应避免陶瓷材料与催化剂间的化学反应导致的催化剂中毒，在选材时也需考虑。
碳化硅蜂窝陶瓷具有优良的常温性能，如优良的抗氧化性、良好的耐腐蚀性、高的抗弯强度以及低的摩擦系数，而且高温性能是已知陶瓷材料中最佳的。碳化硅蜂窝陶瓷在石油、化工、微电子、汽车、航天、航空、造纸、激光、矿业及原子能等工业领域获得了广泛的应用，但是碳化硅由于是共价性极强的化合物，高温烧结困难。
目前，碳化硅蜂窝陶瓷的制备方法有：挤压成型、热压铸成型、注浆成型和添加造孔剂的方法。采用挤压成型方法，由于纯碳化硅浆料的可塑性差而成品率低；采用热压铸成型方法，在烧成过程中，如果升温速率过快或者炉内温度不均匀，制品则会由于排除有机物不均匀而产生裂纹，而要生产高质量的制品则对设备要求过高，生产成本相对过高；采用注浆成型法，虽只需要简单的石膏模具不需要复杂的机械设备，但劳动强度大、操作工序多和生产效率低，且注件含水量高、密度小、收缩大和烧成时容易变形，限制了它的大规模应用；常规的添加造孔剂的方法，无法实现孔径的均匀分布且大小可控，且制品的机械强度一般很差。上述技术缺陷的存在限制了碳化硅蜂窝陶瓷的发展。
发明内容
本发明旨在克服现有技术缺陷，目的是提供一种生产效率高和生产成本低的原位AlN-B4C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、机械强度高和对废气的净化能力强。
为实现上述目的，本发明所采用的技术方案的具体步骤是：
先向主料中加入金属氧化物和结合剂，混合均匀，得到混合料。再将所述混合料倒入真空挤出机中，成型，在60～100℃条件下干燥6～18h，得到蜂窝陶瓷坯体；然后将所述蜂窝陶瓷坯体置入真空热压炉中，在氮气气氛条件下，以4～8℃/min的速率升温至1800～2200℃，保温1～4h，自然冷却，即得原位AlN-B4C增强的碳化硅蜂窝陶瓷。
所述主料是由65～75wt％的粒度为5～50μm的碳化硅粉、20～25wt％的粒度为0.05～0.5μm 的碳化硅粉和3～11wt％的铝硼碳粉混合而成。
所述金属氧化物的加入量为主料的1～5wt％。
所述结合剂是由纤维素、表面活性剂、植物油、甘油和水混合而成：其中：纤维素占所述主料5～6wt％，表面活性剂占所述主料4～6wt％，植物油占所述主料1～4wt％，甘油占所述主料2～5wt％，水为所述纤维素、所述表面活性剂、所述植物油和所述甘油的质量之和。
所述碳化硅粉的纯度为85～99.9％。
所述铝硼碳粉的纯度为95～99.5％；粒度为30～80μm。
所述金属氧化物为氧化铁和氧化镍中的一种以上；纯度为≥98％。
所述纤维素为羟甲基纤维素、乙基纤维素和羟乙基纤维素中的一种以上。
所述表面活性剂为脂肪醇聚氧乙烯醚硫酸铵、月桂醇硫酸钠和十二烷基苯磺酸钠中的一种以上。
所述植物油为樟树油、桉树油和玉桂油中的一种以上。
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：
本发明以两种粒度的碳化硅粉和铝硼碳为主料，其中的碳化硅粉的市场价格低，故生产成本低廉；其制备方法是在主料中加入金属氧化物和结合剂，然后经混合和挤压成型，再经干燥和高温烧结而成，整个工艺流程简单，制品易于成型，过程易于控制，生产效率高。
本发明通过采用添加结合剂与挤压成型相结合的方式，提高混合浆料的可塑性及产品的成品率，也提高了微孔大小和分布的可控性。
本发明向碳化硅粉中加入铝硼碳，在氮气气氛下原位生成AlN-B4C，高温下碳化硼中碳和硼元素固溶到碳化硅晶粒中，占据了碳化硅的中位点，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，提升了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，促使原位 AlN-B4C增强的碳化硅蜂窝陶瓷烧结更为致密，提高了机械性能。
本发明制备的原位AlN-B4C增强的碳化硅蜂窝陶瓷经检测：微孔孔径大小均一，分布均匀，中位孔径为5～15μm；耐压强度为11.8～18.9MPa。
因此，本发明具有生产效率高和生产成本低的特点，用该方法制备的原位AlN-B4C增强的碳化硅蜂窝陶瓷微观结构良好、微孔分布均匀、机械强度高和对废气的净化能力强。
具体实施方案
下面结合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。
为避免重复，先将本具体实施方式所涉及的物料统一描述如下，实施例中不再赘述：
所述碳化硅粉的纯度为85～99.9％。
所述铝硼碳粉的纯度为95～99.5％；粒度为30～80μm。
所述金属氧化物的纯度为≥98％。
实施例1
一种原位AlN-B4C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：
先向主料中加入金属氧化物和结合剂，混合均匀，得到混合料。再将所述混合料倒入真空挤出机中，成型，在60～70℃条件下干燥6～10h，得到蜂窝陶瓷坯体；然后将所述蜂窝陶瓷坯体置入真空热压炉中，在氮气气氛条件下，以4～5℃/min的速率升温至1800～1900℃，保温2.5～3.5h，自然冷却，即得原位AlN-B4C增强的碳化硅蜂窝陶瓷。
所述主料是由65～67wt％的粒度为5～50μm的碳化硅粉、24～25wt％的粒度为0.05～0.5μm 的碳化硅粉和8～11wt％的铝硼碳粉混合而成。
所述金属氧化物的加入量为主料的1～2wt％。
所述结合剂是由纤维素、表面活性剂、植物油、甘油和水混合而成：其中：纤维素占所述主料5～6wt％，表面活性剂占所述主料4～4.5wt％，植物油占所述主料1～2wt％，甘油占所述主料2～3wt％，水为所述纤维素、所述表面活性剂、所述植物油和所述甘油的质量之和。
所述金属氧化物为氧化铁；所述纤维素为羟甲基纤维素；所述表面活性剂为脂肪醇聚氧乙烯醚硫酸铵；所述植物油为樟树油。
本实施例制备的原位AlN-B4C增强的碳化硅蜂窝陶瓷经检测：微孔孔径大小均一，分布均匀，中位孔径为5～15μm；耐压强度为11.8～13.2MPa。
实施例2
一种原位AlN-B4C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：
先向主料中加入金属氧化物和结合剂，混合均匀，得到混合料。再将所述混合料倒入真空挤出机中，成型，在70～80℃条件下干燥8～12h，得到蜂窝陶瓷坯体；然后将所述蜂窝陶瓷坯体置入真空热压炉中，在氮气气氛条件下，以5～6℃/min的速率升温至1900～2000℃，保温1～2h，自然冷却，即得原位AlN-B4C增强的碳化硅蜂窝陶瓷。
所述主料是由67～70wt％的粒度为5～50μm的碳化硅粉、23～24wt％的粒度为0.05～0.5μm 的碳化硅粉和6～10wt％的铝硼碳粉混合而成。
所述金属氧化物的加入量为主料的2～3wt％。
所述结合剂是由纤维素、表面活性剂、植物油、甘油和水混合而成：其中：纤维素占所述主料5～6wt％，表面活性剂占所述主料4.5～5wt％，植物油占所述主料2～3wt％，甘油占所述主料3～4wt％，水为所述纤维素、所述表面活性剂、所述植物油和所述甘油的质量之和。
所述金属氧化物为氧化镍；所述纤维素为乙基纤维素；所述表面活性剂为月桂醇硫酸钠；所述植物油为桉树油。
本实施例制备的原位AlN-B4C增强的碳化硅蜂窝陶瓷经检测：微孔孔径大小均一，分布均匀，中位孔径为5～9μm；耐压强度为12.6～14.4MPa。
实施例3
一种原位AlN-B4C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：
先向主料中加入金属氧化物和结合剂，混合均匀，得到混合料。再将所述混合料倒入真空挤出机中，成型，在80～90℃条件下干燥10～14h，得到蜂窝陶瓷坯体；然后将所述蜂窝陶瓷坯体置入真空热压炉中，在氮气气氛条件下，以6～7℃/min的速率升温至2000～2100℃，保温2～3h，自然冷却，即得原位AlN-B4C增强的碳化硅蜂窝陶瓷。
所述主料是由70～72wt％的粒度为5～50μm的碳化硅粉、22～23wt％的粒度为0.05～0.5μm 的碳化硅粉和5～8wt％的铝硼碳粉混合而成。
所述金属氧化物的加入量为主料的3～4wt％。
所述结合剂是由纤维素、表面活性剂、植物油、甘油和水混合而成：其中：纤维素占所述主料5～6wt％，表面活性剂占所述主料5～5.5wt％，植物油占所述主料3～4wt％，甘油占所述主料4～5wt％，水为所述纤维素、所述表面活性剂、所述植物油和所述甘油的质量之和。
所述金属氧化物为氧化铁和氧化镍中的混合物；所述纤维素为羟乙基纤维素；所述表面活性剂为十二烷基苯磺酸钠；所述植物油为玉桂油。
本实施例制备的原位AlN-B4C增强的碳化硅蜂窝陶瓷经检测：微孔孔径大小均一，分布均匀，中位孔径为8～12μm；耐压强度为13.6～16.7MPa。
实施例4
一种原位AlN-B4C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：
先向主料中加入金属氧化物和结合剂，混合均匀，得到混合料。再将所述混合料倒入真空挤出机中，成型，在90～100℃条件下干燥14～18h，得到蜂窝陶瓷坯体；然后将所述蜂窝陶瓷坯体置入真空热压炉中，在氮气气氛条件下，以7～8℃/min的速率升温至2100～2200℃，保温3～4h，自然冷却，即得原位AlN-B4C增强的碳化硅蜂窝陶瓷。
所述主料是由72～75wt％的粒度为5～50μm的碳化硅粉、20～22wt％的粒度为0.05～0.5μm 的碳化硅粉和3～6wt％的铝硼碳粉混合而成。
所述金属氧化物的加入量为主料的4～5wt％。
所述结合剂是由纤维素、表面活性剂、植物油、甘油和水混合而成：其中：纤维素占所述主料5～6wt％，表面活性剂占所述主料5.5～6wt％，植物油占所述主料3～4wt％，甘油占所述主料3～4wt％，水为所述纤维素、所述表面活性剂、所述植物油和所述甘油的质量之和。
所述金属氧化物为氧化铁；所述纤维素为羟甲基纤维素、乙基纤维素和羟乙基纤维素中的两种以上的混合物；所述表面活性剂为脂肪醇聚氧乙烯醚硫酸铵、月桂醇硫酸钠和十二烷基苯磺酸钠中的两种以上的混合物；所述植物油为樟树油、桉树油和玉桂油中的两种以上的混合物。
本实施例制备的原位AlN-B4C增强的碳化硅蜂窝陶瓷经检测：微孔孔径大小均一，分布均匀，中位孔径为7～11μm；耐压强度为15.8～18.9MPa。
本具体实施方式与现有技术相比具有如下积极效果：
本具体实施方式以两种粒度的碳化硅粉和铝硼碳为主料，其中的碳化硅粉的市场价格低，故生产成本低廉；其制备方法是在主料中加入金属氧化物和结合剂，然后经混合和挤压成型，再经干燥和高温烧结而成，工艺流程简单，制品易于成型，过程易于控制，生产效率高。
本具体实施方式通过采用添加结合剂与挤压成型相结合的方式，提高混合浆料的可塑性及产品的成品率，也提高了微孔大小和分布的可控性。
本具体实施方式向碳化硅粉中加入铝硼碳，在氮气气氛下原位生成AlN-B4C，高温下碳化硼中碳和硼元素固溶到碳化硅晶粒中，占据了碳化硅的中位点，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，提升了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，促使原位AlN-B4C增强的碳化硅蜂窝陶瓷烧结更为致密，提高了机械性能。
本具体实施方式制备的原位AlN-B4C增强的碳化硅蜂窝陶瓷经检测：微孔孔径大小均一，分布均匀，中位孔径为5～15μm；耐压强度为11.8～18.9MPa。
因此，本具体实施方式具有生产效率高和生产成本低的特点，用该方法制备的原位 AlN-B4C增强的碳化硅蜂窝陶瓷微观结构良好、微孔分布均匀、机械强度高和对废气的净化能力强。

Claims (8)

1.一种原位AlN-B4C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：
先向主料中加入金属氧化物和结合剂，混合均匀，得到混合料；再将所述混合料倒入真空挤出机中，成型，在60～100℃条件下干燥6～18h，得到蜂窝陶瓷坯体；然后将所述蜂窝陶瓷坯体置入真空热压炉中，在氮气气氛条件下，以4～8℃/min的速率升温至1800～2200℃，保温1～4h，自然冷却，即得原位AlN-B4C增强的碳化硅蜂窝陶瓷；
所述主料是由65～75wt％的粒度为5～50μm的碳化硅粉、20～25wt％的粒度为0.05～0.5μm的碳化硅粉和3～11wt％的铝硼碳粉混合而成；
所述金属氧化物的加入量为主料的1～5wt％；
所述结合剂是由纤维素、表面活性剂、植物油、甘油和水混合而成：其中：纤维素占所述主料5～6wt％，表面活性剂占所述主料4～6wt％，植物油占所述主料1～4wt％，甘油占所述主料2～5wt％，水为所述纤维素、所述表面活性剂、所述植物油和所述甘油的质量之和。
2.根据权利要求1所述原位AlN-B4C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的纯度为85～99.9％。
3.根据权利要求1所述原位AlN-B4C增强的碳化硅蜂窝陶瓷的制备方法，其特征在于所述铝硼碳粉的纯度为95～99.5％；粒度为30～80μm。
4.根据权利要求1所述原位AlN-B4C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为氧化铁和氧化镍中的一种以上；纯度为≥98％。
5.根据权利要求1所述原位AlN-B4C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为羟甲基纤维素、乙基纤维素和羟乙基纤维素中的一种以上。
6.根据权利要求1所述原位AlN-B4C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为脂肪醇聚氧乙烯醚硫酸铵、月桂醇硫酸钠和十二烷基苯磺酸钠中的一种以上。
7.根据权利要求1所述原位AlN-B4C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为樟树油、桉树油和玉桂油中的一种以上。
8.一种原位AlN-B4C增强的碳化硅蜂窝陶瓷，其特征在于所述原位AlN-B4C增强的碳化硅蜂窝陶瓷是根据权利要求 1～7项中任一项所述原位AlN-B4C增强的碳化硅蜂窝陶瓷的制备方法所制备的原位AlN-B4C增强的碳化硅蜂窝陶瓷。
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