CN105801122B - 一种梯度孔结构碳化硅基多孔陶瓷的制备方法 - Google Patents
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Abstract
本发明属于多孔陶瓷材料的制备领域,具体涉及一种梯度孔结构碳化硅基多孔陶瓷的制备方法。提出的一种梯度孔结构碳化硅基多孔陶瓷的制备方法=采用碳化硅多孔陶瓷作为基体,在碳化硅多孔陶瓷的表面涂覆一层孔径小于碳化硅多孔陶瓷孔径的纳米级氮化硅晶须,形成由内向外孔径逐渐变大的梯度孔结构碳化硅基多孔陶瓷,包括有碳化硅多孔陶瓷的预处理、硅浆的制备、硅浆在碳化硅多孔陶瓷表面的涂覆和气氛烧结四个过程。本发明通过在碳化硅多孔陶瓷的表面涂覆一层孔径小于碳化硅多孔陶瓷孔径的纳米级氮化硅晶须,形成由内向外孔径逐渐变大的梯度孔结构碳化硅基多孔陶瓷,在不降低过滤元件使用性能的前提下提高其耐用性。
Description
技术领域
本发明属于多孔陶瓷材料的制备技术领域,具体涉及一种梯度孔结构碳化硅基多孔陶瓷的制备方法。
背景技术
随着我国工业迅速发展,环境压力越来越大;每当冬季来临,雾霾和PM2.5总能成为人们关注的热点;各种空气净化器的热销也只能在室内的有限空间内起到一定作用;要想根本上缓解和改善大气污染问题,需从工业排放一侧来进行限制和治理;电除尘对微细颗粒的去除率高,但是由于电耗所带来的运行成本很高,受方法限制运行稳度低于350°C;旋风除尘由于运行成本较低而被很多企业所采用;但是旋风除尘对于微细颗粒尤其是粒径在5以下的颗粒,去除效率较低;同时,较低的运行温度也造成了大量的潜热浪费;多孔陶瓷过滤器由于运行温度高,对微细颗粒的去除率高,运行成本较低等优势,正在被更多工业企业所关注和使用。
目前所采用的过滤元件为了保证较高的过滤速率,多孔陶瓷基体通常具有较高的气孔率和较大的气孔孔径;同时,为了提高过滤精度,在多孔陶瓷基体的表面外侧会覆盖一层具有更小孔径的膜结构;在服役过程中,由于长时间的热震、腐蚀、反吹,常常会造成膜结构的破坏和脱落。
发明内容
本发明的目的是提出一种梯度孔结构碳化硅基多孔陶瓷的制备方法,通过在碳化硅多孔陶瓷的表面涂覆一层孔径小于碳化硅多孔陶瓷孔径的纳米级氮化硅晶须,形成由内向外孔径逐渐变大的梯度孔结构碳化硅基多孔陶瓷,在不降低过滤元件使用性能的前提下提高其耐用性。
本发明为完成上述发明目的采用如下技术方案:
一种梯度孔结构碳化硅基多孔陶瓷的制备方法,所述的制备方法采用碳化硅多孔陶瓷作为基体,在碳化硅多孔陶瓷的表面涂覆一层孔径小于碳化硅多孔陶瓷孔径的纳米级氮化硅晶须,形成由内向外孔径逐渐变大的梯度孔结构碳化硅基多孔陶瓷,包括有碳化硅多孔陶瓷的预处理、硅浆的制备、硅浆在碳化硅多孔陶瓷表面的涂覆和气氛烧结四个过程,其具体工艺步骤为:
1)碳化硅多孔陶瓷的预处理:将碳化硅多孔陶瓷置于去离子水中,超声清洗20min,取出后置于烘箱中于100°C烘干24h备用;所述碳化硅多孔陶瓷的气孔率为30~50%,平均孔径为80~200μm;
2)硅浆的制备:将硅粉、分散剂和去离子水置于烧杯中,机械搅拌使其分散均匀得到水基硅浆;所述的硅粉平均粒径在1~20 μm;所述的分散剂为四甲基氢氧化铵或聚乙烯亚胺中的一种;所述的硅粉、分散剂分别为去离子水质量的5~15%,0.3~1.5%;
3)硅浆在碳化硅多孔陶瓷表面的涂覆:将水基硅浆涂覆在碳化硅多孔陶瓷的表面,室温静置,然后置于烘箱中烘干得到碳化硅基多孔陶瓷;
4)气氛烧结:将烘干后的碳化硅基多孔陶瓷置于气氛烧结炉中进行烧结,最终得到具有梯度孔结构的碳化硅基多孔陶瓷。
所述的碳化硅基多孔陶瓷在气氛烧结炉中的烧结过程为,以2-5°C/min的升温速率升至900°C,以0.2-1°C/min的升温速率升至1300-1400°C,保温1-3h后自然降温。
所述的硅浆涂覆可以选择喷涂或刷涂的方式;涂覆后的多孔陶瓷在室温静置24h,然后置于烘箱中于90°C烘干24h。
所述的气氛烧结炉所使用的气氛为氮气。
本发明提出的一种梯度孔结构碳化硅基多孔陶瓷的制备方法,通过在碳化硅多孔陶瓷的表面涂覆一层孔径小于碳化硅多孔陶瓷孔径的纳米级氮化硅晶须,利用硅与氮气之间的氮化反应在碳化硅多孔陶瓷的表面层形成由内向外孔径逐渐变大的梯度孔结构,由于密网结构形成的孔隙很小可以对空气中的微细颗粒物进行有效拦截;同时,密网结构的厚度很薄,由此带来的压力降很小,不会对多孔陶瓷整体的透气率造成明显降低;由于同时具有过滤精度和过滤速率,该梯度孔结构碳化硅基多孔陶瓷可以应用于高温烟尘的过滤领域;在不降低过滤元件使用性能的前提下提高其耐用性。
附图说明
图1所示为实施例1所制备样品的断口形貌照片。
具体实施方式
结合下述实施例及附图对本发明加以说明:
实施例1
选择气孔率为30%,平均孔径为80μm的碳化硅基均匀多孔陶瓷,置于去离子水中,超声清洗20min,取出后于100°C烘干24h。将平均粒径在1 μm的硅粉5g、分散剂TMAH 0.3g和去离子水100g置于烧杯中,机械搅拌得到水基硅浆;将硅浆喷涂或刷涂在碳化硅基均匀多孔陶瓷的表面,室温静置24h,然后于90°C烘干24h;将其转移至气氛烧结炉中进行烧结,通入氮气气氛,以2°C/min的升温速率升至900°C,以1°C/min的升温速率升至1300°C,保温3h后自然降温。所得梯度孔结构碳化硅基多孔陶瓷如图1所示。
实施例2
选择气孔率为37%,平均孔径为160μm的碳化硅基均匀多孔陶瓷,置于去离子水中,超声清洗20min,取出后于100°C烘干24h。将平均粒径在5 μm的硅粉10g、分散剂 PEI 0.6g和去离子水100g置于烧杯中,机械搅拌得到水基硅浆;将硅浆喷涂或刷涂在碳化硅基均匀多孔陶瓷的表面,室温静置24h,然后于90°C烘干24h。将其转移至气氛烧结炉中进行烧结,通入氮气气氛,以5°C/min的升温速率升至900°C,以0.5°C/min的升温速率升至1350°C,保温2h后自然降温。
实施例3
选择气孔率为50%,平均孔径为200μm的碳化硅基均匀多孔陶瓷,置于去离子水中,超声清洗20min,取出后于100°C烘干24h;将平均粒径在20 μm的硅粉15g、分散剂TMAH 1.5g和去离子水100g置于烧杯中,机械搅拌得到水基硅浆。将硅浆喷涂或刷涂在碳化硅基均匀多孔陶瓷的表面,室温静置24h,然后于90°C烘干24h。将其转移至气氛烧结炉中进行烧结,通入氮气气氛,以3°C/min的升温速率升至900°C,以0.2°C/min的升温速率升至1400°C,保温1h后自然降温。
实施例4
选择气孔率为37%,平均孔径为160μm的碳化硅基均匀多孔陶瓷,置于去离子水中,超声清洗20min,取出后于100°C烘干24h。将平均粒径在10 μm的硅粉10g、分散剂 PEI 1.2g和去离子水100g置于烧杯中,机械搅拌得到水基硅浆。将硅浆喷涂或刷涂在碳化硅基均匀多孔陶瓷的表面,室温静置24h,然后于90°C烘干24h。将其转移至气氛烧结炉中进行烧结,通入氮气气氛,以3°C/min的升温速率升至900°C,以0.5°C/min的升温速率升至1370°C,保温2h后自然降温。
Claims (2)
1.一种梯度孔结构碳化硅基多孔陶瓷的制备方法,其特征在于:所述的制备方法采用碳化硅多孔陶瓷作为基体,在碳化硅多孔陶瓷的表面涂覆一层粒径小于碳化硅多孔陶瓷孔径的硅粉,形成由内向外孔径逐渐变小的梯度孔结构碳化硅基多孔陶瓷,包括有碳化硅多孔陶瓷的预处理、硅浆的制备、硅浆在碳化硅多孔陶瓷表面的涂覆和气氛烧结四个过程,其具体工艺步骤为:
1)碳化硅多孔陶瓷的预处理:将碳化硅多孔陶瓷置于去离子水中,超声清洗20min,取出后置于烘箱中于100°C烘干24h备用;所述碳化硅多孔陶瓷的气孔率为30~50%,平均孔径为80~200μm;
2)硅浆的制备:将硅粉、分散剂和去离子水置于烧杯中,机械搅拌使其分散均匀得到水基硅浆;所述的硅粉平均粒径在1~20 μm;所述的分散剂为四甲基氢氧化铵或聚乙烯亚胺中的一种;所述的硅粉、分散剂分别为去离子水质量的5~15%,0.3~1.5%;
3)硅浆在碳化硅多孔陶瓷表面的涂覆:将水基硅浆涂覆在碳化硅多孔陶瓷的表面,室温静置,然后置于烘箱中烘干得到碳化硅基多孔陶瓷;
4)气氛烧结:将烘干后的碳化硅基多孔陶瓷置于气氛烧结炉中进行烧结,最终得到具有梯度孔结构的碳化硅基多孔陶瓷;所述的气氛烧结炉所使用的气氛为氮气;所述的碳化硅基多孔陶瓷在气氛烧结炉中的烧结过程为,以2-5°C/min的升温速率升至900°C,以0.2-1°C/min的升温速率升至1300-1400°C,保温1-3h后自然降温。
2.如权利要求1所述的一种梯度孔结构碳化硅基多孔陶瓷的制备方法,其特征在于:所述的硅浆涂覆可以选择喷涂或刷涂的方式;涂覆后的多孔陶瓷在室温静置24h,然后置于烘箱中于90°C烘干24h。
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