CN108191453A - 一种多孔碳化硅陶瓷及其制备方法 - Google Patents
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Abstract
本发明提供一种多孔碳化硅陶瓷及其制备方法,包括:第一步,造孔剂的制备;第二步,造孔剂与碳化硅粉体球磨;第三步,压制与烧结;第四步,氧化,得到多孔碳化硅陶瓷材料。利用短纤维增韧陶瓷基体烧结制备致密的陶瓷材料,后通过碳纤维的氧化,形成多孔的碳化硅陶瓷。该方法操作简便,流程短,孔隙可控,对制备多孔碳化硅陶瓷材料,特别是孔取向一致的通孔碳化硅陶瓷材料具有十分重要的指导意义。
Description
技术领域
本发明属于多孔材料制备技术领域,涉及一种多孔碳化硅陶瓷的制备方法。
背景技术
多孔碳化硅陶瓷由于具有低密度、耐高温、耐腐蚀、抗氧化与抗热震性等特点,广泛应用于高温气体过滤材料、催化剂载体与耐火材料领域。目前,已经较多应用的是多孔陶瓷多为氧化物陶瓷,但其存在高温性能不佳与耐腐蚀性能不足等缺点,而多孔碳化硅具有比氧化物陶瓷更好的性能而应用于高温领域,关于多孔碳化硅陶瓷的制备成为目前研究的热点之一。
CN102807391B公开了一种多孔碳化硅陶瓷的制备方法,包括:制备浆料;二制备孔陶瓷生坯;制备预制体;制备碳凝胶;制备多孔碳化硅与碳凝胶的复合材料;制备多孔碳化硅和炭气凝胶的复合材料;将多孔碳化硅和炭气凝胶的复合材料与单质硅粉放入烧结炉中烧结,即得多孔碳化硅陶瓷。
CN104402446A了公开了一种制备多孔碳化硅陶瓷的方法,包括以碱性硅溶胶与碳化硅陶瓷粉体球磨混合配制成碳化硅陶瓷水基悬浮料浆;加入表面活性剂,悬浮料浆经搅拌发泡至设计倍率;再加入促凝剂,并搅拌均匀;将料浆注入非吸水模具中,碱性硅溶胶在促凝剂的作用下凝胶固化;脱模干燥后,将坯体渗入一定量的含C源的液体溶液;待溶剂挥发后,坯体经高温氩气保护反应烧结制得多孔碳化硅陶瓷。
CN105541370A公开了多孔碳化硅陶瓷材料的制备方法,包括:制备活性铝硅酸盐源材料;制备球磨混合物;制备碱激发溶液;制备无机聚合物配合料;制备胚料;高温处理,得到多孔碳化硅陶瓷材料。
CN105294107A公开了一种多孔碳化硅陶瓷及其制备方法,该制备方法包括如下步骤:将碳化硅、氢氧化铝、气相白炭黑、水、分散剂和粘结剂混合,得到浆料,其中,氢氧化铝与所述气相白炭黑的质量之和占碳化硅、所述氢氧化铝和气相白炭黑的质量之和的5~30%,且氢氧化铝与气相白炭黑的摩尔比为2~5:1;将浆料干燥,得到混合粉体;将混合粉体成型,得到生坯;在空气气氛下,将生坯于1310~1340℃烧结,得到多孔碳化硅陶瓷。采用上述制备方法能够在较低的烧结温度下制备出抗弯较好的多孔碳化硅陶瓷。
以上专利及公知技术生产的多孔碳化硅陶瓷主要是采用溶液制备浆料,流程长,孔结构与分布受到工艺参数的严重影响。
发明内容
针对现有多孔碳化硅陶瓷制备方法存在的不足,本发明提供一种多孔碳化硅陶瓷的制备方法,操作简便,准确度高,孔结构可控。
为了实现上述目的,本发明所述的一种多孔碳化硅陶瓷的制备方法,包括以下步骤:
第一步,造孔剂的制备;
按重量份,将100份碳纤维,0.1-1份硼烷异戊基硫化物络合物,1-10份ε-己内酰胺与亚胺基六次甲基亚胺基己二酰的聚合物,0.5-2份1-芘癸酸,300-800份甲苯,70-90℃,反应1-5小时,过滤,烘干,得到造孔剂;
第二步,湿磨,将短纤维与碳化硅粉体加入球磨罐中,球磨比为5-10,加入酒精进行球磨,转速为30-100r/min,时间为5-20h。
第三步中,冷等静压压制,毛坯的致密度为70-90%,再经放电等离子烧结,烧结温度为1600-2000℃,时间为10-30min。
第四步中,氧化烧结,气氛为氢气,烧结温度为600-800℃,时间为3-6h。
优选地,第一步中,所述的碳纤维裁剪成长度为1-3mm的短纤维。
本发明方法的原理:上述的一种多孔碳化硅陶瓷的制备方法,将碳化硅粉体与造孔剂球磨混合均匀,得到复合粉体,压制后在高温下烧结成致密的碳纤维增韧碳化硅陶瓷材料;利用碳纤维的氧化性质,使碳纤维在高温下氧化,形成多孔碳化硅陶瓷材料。通过调节碳纤维的长度与含量,可调控孔的数量与发布,甚至是孔取向一致的通孔碳化硅陶瓷材料。
因此,本发明方法对制备多孔碳化硅陶瓷材料具有十分重要的指导意义。
具体实施方式
下面结合具体实施例对本发明进行详细说明。以下实施例将有助于本领域的技术人员进一步理解本发明,但不以任何形式限制本发明。应当指出的是,对本领域的普通技术人员来说,在不脱离本发明构思的前提下,还可以做出若干变形和改进。这些都属于本发明的保护范围。
实施例1:
按重量份,将100份碳纤维,0.3份硼烷异戊基硫化物络合物,4份ε-己内酰胺与亚胺基六次甲基亚胺基己二酰的聚合物,1份1-芘癸酸,500份甲苯,80℃,反应2小时,过滤,烘干,得到造孔剂;
将造孔剂与50%粒径为10-30μm的碳化硅粉体加入球磨罐中,加入60%酒精,球料比为5:1,球磨转速为40r/min,时间为10h后分离与干燥粉体得到复合粉体;将复合粉体压制成致密度为75%的坯体;将毛坯进行放电等离子烧结,烧结温度为1700℃下烧结15min得到碳化硅陶瓷,然后在氢气气氛中进行氧化烧结,烧结参数为600℃与5h,得到多孔碳化硅陶瓷材料。样品编号为C-1。
实施例2:
按重量份,将100份碳纤维,0.1份硼烷异戊基硫化物络合物,1份ε-己内酰胺与亚胺基六次甲基亚胺基己二酰的聚合物,0.5份1-芘癸酸,300份甲苯,70℃,反应1小时,过滤,烘干,得到造孔剂;
将造孔剂与40%粒径为40-70μm的碳化硅粉体加入球磨罐中,加入70%酒精,球料比为6:1,球磨转速为45r/min,时间为12h后分离与干燥粉体得到复合粉体;将复合粉体压制成致密度为80%的坯体;将毛坯进行放电等离子烧结,烧结温度为1750℃下烧结15min得到碳化硅陶瓷,然后在氢气气氛中进行氧化烧结,烧结参数为650℃与5h,得到多孔碳化硅陶瓷材料。样品编号为C-2。
实施例3:
按重量份,将100份碳纤维,1份硼烷异戊基硫化物络合物,10份ε-己内酰胺与亚胺基六次甲基亚胺基己二酰的聚合物,2份1-芘癸酸,800份甲苯,90℃,反应5小时,过滤,烘干,得到造孔剂;
将造孔剂与40%粒径为10-30μm的碳化硅粉体加入球磨罐中,加入75%酒精,球料比为5:1,球磨转速为50r/min,时间为11h后分离与干燥粉体得到复合粉体;将复合粉体压制成致密度为86%,的坯体;将毛坯进行放电等离子烧结,烧结温度为1850℃下烧结15min得到碳化硅陶瓷,然后在氢气气氛中进行氧化烧结,烧结参数为750℃与4h,得到多孔碳化硅陶瓷材料。样品编号为C-3。
对比例1:
不加入硼烷异戊基硫化物络合物,其他和实施例1一致。样品编号为C-4。
对比例2:
不加入ε-己内酰胺与亚胺基六次甲基亚胺基己二酰的聚合物,其他和实施例1一致。样品编号为C-5。
对比例3:
不进行氧化烧结,其他和实施例1一致。样品编号为C-6。
将制备的多孔碳化硅陶瓷材料按GB/T19744进行制样,将断口进行扫描电镜形貌检测,测量10组不同区域2000×下的孔结构,统计通孔占孔百分比;通过阿基米德原理来计算多孔碳化硅的孔隙,数据如下表所示。
表:本发明制备的多孔碳化硅的孔隙与通孔对比。
样品编号 | 多孔碳化硅孔隙 % | 多孔碳化硅通孔百分比 % |
C-1 | 49.8 | 32.3 |
C-2 | 43.6 | 30.1 |
C-3 | 42.1 | 28.6 |
C-4 | 2.5 | 0.6 |
C-5 | 23.3 | 13.6 |
C-6 | 1.8 | 0.1 |
通过上述实施例可以看出,本发明方法能够有效地可控制备多孔碳化硅陶瓷,解决了现有技术中的不足,流程短,操作简单快捷孔隙可控,这对制备多孔碳化硅陶瓷材料具有十分重要的指导意义。
以上对本发明的具体实施例进行了描述。需要理解的是,本发明并不局限于上述特定实施方式,本领域技术人员可以在权利要求的范围内做出各种变形或修改,这并不影响本发明的实质内容。
Claims (5)
1.一种多孔碳化硅陶瓷及其制备方法,其特征在于,包括以下步骤:
第一步,造孔剂的制备;
按重量份,将100份碳纤维,0.1-1份硼烷异戊基硫化物络合物,1-10份ε-己内酰胺与亚胺基六次甲基亚胺基己二酰的聚合物,0.5-2份1-芘癸酸,300-800份甲苯,70-90℃,反应1-5小时,过滤,烘干,得到造孔剂;
第二步,湿磨,将短纤维与碳化硅粉体加入球磨罐中,球磨比为5-10,加入酒精进行球磨,转速为30-100r/min,时间为5-20h;
第三步中,冷等静压压制,毛坯的致密度为70-90%,再经放电等离子烧结,烧结温度为1600-2000℃,时间为10-30min;
第四步中,氧化烧结,气氛为氢气,烧结温度为600-800℃,时间为3-6h。
2.如权利要求1所述的一种多孔碳化硅陶瓷及其制备方法,其特征在于,第一步中,所述的造孔剂为碳纤维,将碳纤维裁剪成长度为1-3mm的短纤维。
3.如权利要求1所述的一种多孔碳化硅陶瓷及其制备方法,其特征在于,第二步中,所述球磨为湿磨,将短纤维与碳化硅粉体加入球磨罐中,球磨比为5-10,加入酒精进行球磨,转速为30-100r/min,时间为5-20h。
4.如权利要求1所述的一种多孔碳化硅陶瓷及其制备方法,其特征在于,第三步中,所述压制为冷等静压压制,毛坯的致密度为70-90%;所述烧结为放电等离子烧结,烧结温度为1600-2000℃,时间为10-30min。
5.如权利要求1所述的一种多孔碳化硅陶瓷及其制备方法,其特征在于,第四步中,所述氧化为氧化烧结,气氛为氢气,烧结温度为600-800℃,时间为3-6h。
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CN111233457A (zh) * | 2020-01-19 | 2020-06-05 | 陕西科技大学 | 一种基于碳纤维为造孔剂和增强体制备多孔镁掺杂ha基复合材料的方法 |
CN111848158A (zh) * | 2020-06-18 | 2020-10-30 | 日照鼎源新材料有限公司 | 湿纺共挤出制备具有致密孔壁的直通孔氧化锆陶瓷的方法 |
CN111848208A (zh) * | 2020-06-18 | 2020-10-30 | 日照鼎源新材料有限公司 | 湿纺共挤出制备具有致密孔壁的直通孔氧化锆陶瓷 |
CN111875407A (zh) * | 2020-06-18 | 2020-11-03 | 日照鼎源新材料有限公司 | 湿纺共挤出制备具有致密孔壁的直通孔氧化铝陶瓷 |
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2018
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
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CN111233457A (zh) * | 2020-01-19 | 2020-06-05 | 陕西科技大学 | 一种基于碳纤维为造孔剂和增强体制备多孔镁掺杂ha基复合材料的方法 |
CN111233457B (zh) * | 2020-01-19 | 2022-02-08 | 陕西科技大学 | 一种基于碳纤维为造孔剂和增强体制备多孔镁掺杂ha基复合材料的方法 |
CN111848158A (zh) * | 2020-06-18 | 2020-10-30 | 日照鼎源新材料有限公司 | 湿纺共挤出制备具有致密孔壁的直通孔氧化锆陶瓷的方法 |
CN111848208A (zh) * | 2020-06-18 | 2020-10-30 | 日照鼎源新材料有限公司 | 湿纺共挤出制备具有致密孔壁的直通孔氧化锆陶瓷 |
CN111875407A (zh) * | 2020-06-18 | 2020-11-03 | 日照鼎源新材料有限公司 | 湿纺共挤出制备具有致密孔壁的直通孔氧化铝陶瓷 |
CN111848158B (zh) * | 2020-06-18 | 2022-10-04 | 日照鼎源新材料有限公司 | 湿纺共挤出制备具有致密孔壁的直通孔氧化锆陶瓷的方法 |
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