CN110357655B - 一种仿生结构碳化硅基多孔陶瓷及其制备方法 - Google Patents

一种仿生结构碳化硅基多孔陶瓷及其制备方法 Download PDF

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CN110357655B
CN110357655B CN201910665849.3A CN201910665849A CN110357655B CN 110357655 B CN110357655 B CN 110357655B CN 201910665849 A CN201910665849 A CN 201910665849A CN 110357655 B CN110357655 B CN 110357655B
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徐晓虹
刘星
吴建锋
张亚祥
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Wuhan University of Technology WUT
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Abstract

本发明涉及一种仿生结构碳化硅基多孔陶瓷及其制备方法，上述制备方法包括：将陶瓷骨料球磨后过筛，取粒径为88‑150μm颗粒备用；将结合剂球磨后过250目筛，再向过筛后颗粒中混入矿化剂，得粘结剂，备用；取76‑82wt％陶瓷骨料、18‑24wt％粘结剂，将其球磨混合均匀后再向其中加入造孔剂并球磨混合均匀，得坯料；将坯料陈腐一段时间后于模具中压制形成坯体，再将坯体干燥后烧制，即可获得一种仿生结构碳化硅基多孔陶瓷。本发明提供的仿生结构碳化硅基多孔陶瓷为单层结构，避免了常规设计中因涂覆膜层而需二次烧成的技术问题，相应的其也可避免膜层在使用过程中易脱落等问题，因而整体使用寿命长。

Description

一种仿生结构碳化硅基多孔陶瓷及其制备方法
技术领域
本发明涉及高温除尘用多孔陶瓷技术领域，尤其涉及一种仿生结构碳化硅基多孔陶瓷及其制备方法。
背景技术
碳化硅基多孔陶瓷因强度高、抗氧化性和抗热震性较好、导热性好、耐腐蚀等优点广泛应用于高温气固分离、金属熔融过滤、催化剂载体等领域。目前常见的制备多孔陶瓷的方法有颗粒堆积法、添加造孔剂法以及晶须堆积等。中国发明专利《一种纯质碳化硅过滤膜层》(CN102659447B)公开了一种采用颗粒堆积以及添加造孔剂来制备纯质碳化硅多孔陶瓷过滤膜层的方法，该方法制备的碳化硅膜层孔径为0.1～20μm，气孔率为25～50％。中国发明专利《一种高孔隙率莫来石晶须多孔陶瓷管及制备方法》(CN107721448A)公开了一种由均匀莫来石晶须互锁形成的高孔隙率多孔陶瓷管及其制备方法，该方法制备的莫来石晶须多孔陶瓷管气孔率大于70％，抗折强度大于3MPa。上述采用颗粒堆积法、添加造孔剂法或晶须堆积形成的多孔陶瓷虽然气孔率较高，但气孔孔径较小，抗折强度较低，不利于多孔陶瓷高效过滤以及长期使用。
仿生材料是模仿自然界生物的结构来实现某种特定功能的新材料。人体支气管因其内壁表面长有大量纤毛而具有捕获空气中微小灰尘及细菌的能力。因此，如果仿照人体支气管纤毛结构设计制备多孔陶瓷材料，就可以实现其高效精细过滤分离有害粉尘的目的。
发明内容
针对上述问题，现提供一种仿生结构碳化硅基多孔陶瓷及其制备方法，旨在提供一种孔径较大、抗折强度较高、气孔率较大的仿生结构碳化硅基多孔陶瓷，该陶瓷可对800℃以上高温烟尘实现高效精细过滤。
具体技术方案如下：
本发明的第一个方面是提供一种仿生结构碳化硅基多孔陶瓷的制备方法，具有这样的特征，包括如下步骤：
步骤一、将陶瓷骨料球磨后过筛，取粒径为88-150μm颗粒备用；将结合剂球磨后过250目筛，再向过筛后颗粒中混入矿化剂，得粘结剂，备用；
步骤二、以坯料质量计取76-82％陶瓷骨料、18-24％粘结剂，以陶瓷骨料质量计取5-10％聚乙烯醇溶液，将三者球磨混合均匀后再向其中加入造孔剂并球磨混合均匀，得坯料；
步骤三：将坯料陈腐一段时间后于模具中压制形成坯体，再将坯体干燥后烧制，即可获得一种仿生结构碳化硅基多孔陶瓷；
其中，陶瓷骨料为碳化硅，矿化剂为MoO3。
上述的制备方法，还具有这样的特征，步骤一中结合剂由高岭土和α-Al2O3按质量比为(62-78):(22-38)混合形成。
上述的制备方法，还具有这样的特征，高岭土的成分为SiO2 45-53wt％、Al2O3 30-38wt％、Fe2O3 2-3wt％、TiO2 0-1wt％、CaO 0-1wt％、MgO 0-1wt％、K2O 0-1wt％，且上述高岭土的烧失量为2-21％。
上述的制备方法，还具有这样的特征，步骤一中以结合剂质量计矿化剂的加入量为12.5-62.5％。
上述的制备方法，还具有这样的特征，步骤二中聚乙烯醇溶液的质量分数为2-5％。
上述的制备方法，还具有这样的特征，步骤二中造孔剂由石墨和活性炭按任意质量比混合形成，且以陶瓷骨料及结合剂质量和计其加入量为20-30％。
上述的制备方法，还具有这样的特征，石墨及活性炭粒径均为100-200μm。
上述的制备方法，还具有这样的特征，步骤三中压制压力为30-50MPa；干燥温度为70-90℃，干燥时间为18-24h。
上述的制备方法，还具有这样的特征，步骤三中烧制温度为1350-1500℃，烧制方法为：当温度＜1000℃时，升温速率为5℃/min，并每升温100℃保温30min；当温度≥1000℃时，升温速率为3℃/min，并每升温100℃保温60min；当温度达到最高温度后保温2-4h。
本发明的第二个方面是提供一种仿生结构碳化硅基多孔陶瓷，具有这样的特征，根据上述制备方法制备获得。
上述方案的有益效果是：
1)、本发明提供的仿生结构碳化硅基多孔陶瓷因孔径较大(平均孔径为83.23-183.52μm)，因而在无需涂覆分离膜层的情况下即可实现对800℃以上高温烟尘的高效过滤，测试表明，其过滤速率达250m3/(m2·h·kPa)以上；且由于孔道内壁晶须的存在对含尘烟气具有过滤作用，加之气孔孔径较大(平均孔径为83.23-183.52μm)，从而在实现高效过滤的同时实现对含尘烟气的精细过滤，测试表明，其对PM2.5的过滤精度达99.99％以上；
2)、本发明提供的仿生结构碳化硅基多孔陶瓷为单层结构，避免了常规设计中因涂覆膜层而需二次烧成的技术问题，相应的其也可避免膜层在使用过程中易脱落等问题，因而整体使用寿命长；
3)、本发明提供的制备方法工序简单、成本低且能耗少。
附图说明
图1为本发明的实施例1中提供的仿生结构碳化硅基多孔陶瓷的孔道(a)及孔道内壁(b)的显微结构图；
图2为本发明的实施例1中提供的仿生结构碳化硅基多孔陶瓷在低倍镜下的显微结构图。
具体实施方式
下面将结合本发明实施例中的附图，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有作出创造性劳动的前提下所获得的所有其他实施例，都属于本发明保护的范围。
需要说明的是，在不冲突的情况下，本发明中的实施例及实施例中的特征可以相互组合。下面结合附图和具体实施例对本发明作进一步说明，但不作为本发明的限定。
实施例1
一种仿生结构碳化硅基多孔陶瓷，其制备方法为：将碳化硅骨料球磨后过筛，取粒径为88-150μm颗粒备用；将结合剂(由高岭土和α-Al2O3按质量比62:38混合形成)球磨后过250目筛，再向过筛后颗粒中混入12.5wt％的MoO3，得粘结剂，备用；以坯料质量计取76％陶瓷骨料、24％粘结剂，以陶瓷骨料质量计取5％聚乙烯醇溶液(质量分数为2％)，将陶瓷骨料、粘结剂及聚乙烯醇溶液混合并球磨30min使其混合均匀，再向其中加入造孔剂(由粒径为100μm的石墨及粒径为100μm的活性炭按任意质量比混合形成，且以碳化硅骨料及结合剂质量和计其加入量为20％)并球磨混合30min使其混合均匀，得坯料；将坯料陈腐24h后于模具中在30MPa下压制形成坯体，再将坯体于70℃下干燥为24h后进行烧制，烧制温度为1500℃，烧制方法为：当温度＜1000℃时，升温速率为5℃/min，并每升温100℃保温30min；当温度≥1000℃时，升温速率为3℃/min，并每升温100℃保温60min；当温度达到1500℃后保温4h，烧制完成后冷却至室温，即可获得一种仿生结构碳化硅基多孔陶瓷。
如图1所示，本实施例提供的仿生结构碳化硅基多孔陶瓷中存在大量气孔，且气孔之间有相互连通的孔道，同时，孔道内壁生长有大量晶须(研究表明，这些晶须的存在对提高过滤精度有促进作用)。
低倍显微镜下观察表明，本实施例提供的仿生结构碳化硅基多孔陶瓷中气孔平均孔径为83.23μm(如图2所示)。
测试表明，本实施例中制备的仿生结构碳化硅基多孔陶瓷的气孔率为42.32％，抗折强度为23.10MPa，过滤速率为264m3/(m2·h·kPa)，对PM2.5的过滤精度达99.99％。
实施例2
一种仿生结构碳化硅基多孔陶瓷，其制备方法为：将碳化硅骨料球磨后过筛，取粒径为88-150μm颗粒备用；将结合剂(由高岭土和α-Al2O3按质量比70:30混合形成)球磨后过250目筛，再向过筛后颗粒中混入47wt％的MoO3，得粘结剂，备用；以坯料质量计取79％陶瓷骨料、21％粘结剂，以陶瓷骨料计取8％聚乙烯醇溶液(质量分数为3.5％)，将陶瓷骨料、粘结剂及聚乙烯醇溶液混合并球磨40min使其混合均匀，再向其中加入造孔剂(由粒径为150μm的石墨及粒径为150μm的活性炭按任意质量比混合形成，且以碳化硅骨料及结合剂质量和计其加入量为25％)并球磨混合45min使其混合均匀，得坯料；将坯料陈腐36h后于模具中在40MPa下压制形成坯体，再将坯体于75℃下干燥为22h后进行烧制，烧制温度为1400℃，烧制方法为：当温度＜1000℃时，升温速率为5℃/min，并每升温100℃保温30min；当温度≥1000℃时，升温速率为3℃/min，并每升温100℃保温60min；当温度达到1400℃后保温3h，烧制完成后冷却至室温，即可获得一种仿生结构碳化硅基多孔陶瓷。
低倍显微镜下观察表明，本实施例提供的仿生结构碳化硅基多孔陶瓷中气孔平均孔径为142.65μm。
测试表明，本实施例中制备的仿生结构碳化硅基多孔陶瓷的气孔率为43.26％，，抗折强度为21.14MPa，过滤速率为295m3/(m2·h·kPa)，对PM2.5的过滤精度达99.99％。
实施例3
一种仿生结构碳化硅基多孔陶瓷，其制备方法为：将碳化硅骨料球磨后过筛，取粒径为88-150μm颗粒备用；将结合剂(由高岭土和α-Al2O3按质量比78:22混合形成)球磨后过250目筛，再向过筛后颗粒中混入62.5wt％的MoO3，得粘结剂，备用；以坯料质量计取82％陶瓷骨料、18％粘结剂，以陶瓷骨料计取10％聚乙烯醇溶液(质量分数为5％)，将陶瓷骨料、粘结剂及聚乙烯醇溶液混合并球磨60min使其混合均匀，再向其中加入造孔剂(由粒径为200μm的石墨及粒径为200μm的活性炭按任意质量比混合形成，且以碳化硅骨料及结合剂质量和计其加入量为25％)并球磨混合60min使其混合均匀，得坯料；将坯料陈腐48h后于模具中在50MPa下压制形成坯体，再将坯体于90℃下干燥为18h后进行烧制，烧制温度为1350℃，烧制方法为：当温度＜1000℃时，升温速率为5℃/min，并每升温100℃保温30min；当温度≥1000℃时，升温速率为3℃/min，并每升温100℃保温60min；当温度达到1350℃后保温2h，烧制完成后冷却至室温，即可获得一种仿生结构碳化硅基多孔陶瓷。
低倍显微镜下观察表明，本实施例提供的仿生结构碳化硅基多孔陶瓷中气孔平均孔径为183.52μm。
测试表明，本实施例中制备的仿生结构碳化硅基多孔陶瓷的气孔率为45.12％，抗折强度为19.73MPa，过滤速率为364m3/(m2·h·kPa)，对PM2.5的过滤精度达99.99％。
以上仅为本发明较佳的实施例，并非因此限制本发明的实施方式及保护范围，对于本领域技术人员而言，应当能够意识到凡运用本发明说明书及图示内容所作出的等同替换和显而易见的变化所得到的方案，均应当包含在本发明的保护范围内。

Claims (5)

1.一种仿生结构碳化硅基多孔陶瓷的制备方法，其特征在于，包括如下步骤：
步骤一、将陶瓷骨料球磨后过筛，取粒径为88-150 μm颗粒备用；将结合剂球磨后过250目筛，再向过筛后颗粒中混入矿化剂，得粘结剂，备用；
步骤二、以坯料质量计取76-82 %陶瓷骨料、18-24 %粘结剂，以所述陶瓷骨料质量计取5-10 %聚乙烯醇溶液，将三者球磨混合均匀后再向其中加入造孔剂并球磨混合均匀，得坯料；
步骤三：将坯料陈腐一段时间后于模具中压制形成坯体，再将坯体干燥后烧制，即可获得一种仿生结构碳化硅基多孔陶瓷；
其中，所述陶瓷骨料为碳化硅，所述矿化剂为MoO3；步骤一中所述结合剂由高岭土和α-Al2O3按质量比为(62-78) : (22-38)混合形成；步骤一中以结合剂质量计所述矿化剂的加入量为12.5-62.5 %；步骤二中所述造孔剂由粒径均为100-200 μm石墨和活性炭按任意质量比混合形成，且以所述陶瓷骨料及所述结合剂质量和计其加入量为20-30 %；步骤三中烧制温度为1350-1500 ℃，烧制方法为：当温度＜1000 ℃时，升温速率为5 ℃/min，并每升温100 ℃保温30 min；当温度≥1000 ℃时，升温速率为3 ℃/min，并每升温100 ℃保温60min；当温度达到最高温度后保温2-4h。
2.根据权利要求1所述的制备方法，其特征在于，所述高岭土的成分为SiO2 45-53 wt%、Al2O3 30-38 wt%、Fe2O3 2-3 wt%、TiO2 0-1 wt%、CaO 0-1 wt%、MgO 0-1 wt%、K2O 0-1 wt%，且其烧失量为2-21 %。
3.根据权利要求1所述的制备方法，其特征在于，步骤二中聚乙烯醇溶液的质量分数为2-5 %。
4.根据权利要求1所述的制备方法，其特征在于，步骤三中压制压力为30-50 MPa；干燥温度为70-90 ℃，干燥时间为18-24 h。
5.一种仿生结构碳化硅基多孔陶瓷，其特征在于，根据权利要求1-4任一项所述制备方法制备获得。
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