CN106007763A - 一种制备全晶须结构莫来石蜂窝陶瓷载体的方法 - Google Patents
一种制备全晶须结构莫来石蜂窝陶瓷载体的方法 Download PDFInfo
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Abstract
本发明属于无机材料技术领域，具体涉及一种制备全晶须结构莫来石蜂窝陶瓷载体的方法。提出的一种制备全晶须结构莫来石蜂窝陶瓷载体的方法以壳聚糖为有机聚合单体，采用戊二醛作为引发剂结合莫来石晶须原位生长技术来制备莫来石蜂窝陶瓷载体，得到全部由原位生长的晶须构成的莫来石蜂窝陶瓷块体材料，其具体步骤为1）陶瓷浆料的制备,2）浆料的固化成型，3）样品的烘干和坯体的烧结。本发明可以通过改变陶瓷浆料的固含量来调节孔隙率；整个陶瓷块体由原位生长的莫来石晶须构成，力学性能好。
Description
技术领域
本发明属于无机非金属材料技术领域，具体涉及一种制备全晶须结构莫来石蜂窝陶瓷载体的方法。
背景技术
凝胶注模工艺是由美国橡树岭国家实验室开发的陶瓷成型工艺，该工艺可以在烧结前对样品进行任意成型凝胶注模工艺开发的目的是用来制备致密陶瓷，该工艺后来也开始应用于多孔陶瓷的成型。如马艺娟等（中国专利，公开号CN105481466A）利用凝胶注模工艺制备多孔磷酸钙生物陶瓷材料；贾留宽等（中国专利，公开号CN105294111A）利用凝胶注模工艺制备高孔隙率的氮化硅多孔陶瓷。凝胶注模工艺是将陶瓷粉料混合聚合物单体配制成陶瓷浆料，然后加入交联剂，使聚合物单体交联成三维网络，将陶瓷粉原位固化，然后再经过排胶和烧结得到致密或是多孔陶瓷。传统的凝胶注模用的有机单体一般为丙烯酰胺，该有机单体有毒，对环境危害较大。壳聚糖也可以作为凝胶注模成型的有机聚合单体，壳聚糖主链上的胺基可以与含羰基的化合物发生缩聚反应，形成交联网络结构从而对陶瓷浆料起到固化作用。利用壳聚糖作为有机聚合单体的优点主要是无毒环保，不需要升温在常温下既可以快速固化。
发明内容
针对上述技术现状，本发明的目的是提出一种制备全晶须结构莫来石蜂窝陶瓷载体的方法，本发明利用新型的凝胶注模技术和莫来石晶须的原位生长技术来制备高孔隙率和孔径分布可控的全晶须结构的莫来石蜂窝陶瓷载体。
本发明为完成上述目的采用如下技术方案：
一种基于新型凝胶注模工艺制备蜂窝陶瓷载体的方法，所述的制备方法以壳聚糖为有机聚合单体，戊二醛作为引发剂，氧化铝和二氧化硅作为莫来石前驱体粉末，外加晶须生长助剂，得到全部由莫来石晶须构成的蜂窝陶瓷块体材料，其具体步骤如下：
1）陶瓷浆料的制备：氧化铝、二氧化硅和晶须生长助剂按照65～78wt%：21～26wt% ：1～10wt%的重量比加入到水中，再加入占粉体总质量0.5 wt %的壳聚糖作为有机聚合单体配成固含量为40～70 wt %的陶瓷浆料，并在所述的陶瓷浆料中加入醋酸，使陶瓷浆料的PH值为1.5 ～5；
2） 浆料的固化成型：将步骤1）所制备的陶瓷浆料倒入模具中并加入占陶瓷浆料总质量0.6%的戊二醛作为引发剂，然后在常温下静置0.5～5小时固化成型；
3）样品的烘干：将样品脱模后在40～80℃烘干5～20小时得到陶瓷坯体；
4）坯体的烧结：将步骤3）烘干得到的陶瓷坯体置于马弗炉中以1～10℃/min升温至1000℃，保温0～3小时后，再以1～7℃/min 继续升温至1200～1600℃保温1～5小时使坯体烧结，然后随炉冷却，得到主晶相为莫来石相的全晶须结构莫来石蜂窝陶瓷载体。
所述的晶须生长助剂为氟化铝、五氧化二钒、三氧化钼中的一种或几种的混合。
所述的莫来石蜂窝陶瓷载体具有原位生长的晶须结构。
所述莫来石蜂窝陶瓷载体的显气孔率为50%～83%。
所述莫来石蜂窝陶瓷载体的抗压强度为5～80MPa。
本发明提出的一种制备全晶须结构莫来石蜂窝陶瓷载体的方法，采用壳聚糖作为凝胶注模成型的有机聚合单体，壳聚糖主链上的胺基可以与含羰基的化合物发生缩聚反应，形成交联网络结构从而对陶瓷浆料起到固化作用；利用壳聚糖作为有机聚合单体的优点主要是无毒环保，不需要升温在常温下既可以快速固化；另外可以按照模具的形状自由成型，也不需要复杂的排胶过程，是一种非常有应用前景的全晶须结构莫来石蜂窝陶瓷载体制备方法；本发明可以通过改变陶瓷浆料的固含量来调节孔隙率； 整个陶瓷块体由原位生长的莫来石晶须构成，力学性能好。
附图说明
图1为1500℃保温2h的莫来石多孔陶瓷的XRD图谱；横坐标为二倍衍射角，单位为度，纵坐标为衍射强度的相对值。
图2为实施例1中1500℃保温两小时烧结得到的全晶须结构莫来石多孔陶瓷的扫描电镜(SEM)形貌。
图3为实施例2中1500℃保温两小时烧结得到的全晶须结构莫来石多孔陶瓷的扫描电镜(SEM)形貌。
具体实施方式
下面结合附图和具体实施例对本发明加以说明，但本发明并不局限于实施例。
实施例1：向200ml水中加入200g陶瓷粉体，其中Al2O3、二氧化硅、氟化铝和三氧化钼的质量比为68:26:3:3；并加入占粉体总质量0.5wt%的壳聚糖，将得到的混合物于常温下用磁力搅拌器搅拌30min，得到均匀分散的陶瓷浆料；向陶瓷浆料中加入醋酸调节PH值为1.5，再将陶瓷浆料倒入模具中,并加入占陶瓷浆料总质量0.6wt%的戊二醛作为引发剂于常温下静置经0.5小时固化成型后脱模，脱模后的样品在烘箱中于60℃烘干12小时, 再移入马弗炉中以5℃/min速率升温至1500℃，保温2h；得到的全晶须结构莫来石多孔陶瓷微观结构如附图2；1500℃保温2h的莫来石蜂窝陶瓷载体的XRD图谱见图1。
实施例2：向200ml水中加入300g陶瓷粉体，其中Al2O3、二氧化硅、氟化铝和五氧化二钒的质量比为68:26:3:3；并加入占粉体总质量0.5wt%的壳聚糖，将得到的混合物于常温下用磁力搅拌器搅拌30min，得到均匀分散的陶瓷浆料；向陶瓷浆料中加入醋酸调节PH值为2，再将陶瓷浆料倒入模具中,并加入占陶瓷浆料0.6wt%的戊二醛作为引发剂于常温下静置经1小时固化成型后脱模，脱模后的样品在烘箱中于60℃烘干12小时, 再移入马弗炉中以5℃/min速率升温至1500℃，保温2h；得到的全晶须结构莫来石多孔陶瓷微观结构如附图3，1500℃保温2h的莫来石蜂窝陶瓷载体的XRD图谱见图1。
实施例3：向200ml水中加入300g陶瓷粉体，其中Al2O3、二氧化硅、氟化铝质量比为73:21:6；并加入占粉体总质量0.5wt%的壳聚糖，将得到的混合物于常温下用磁力搅拌器搅拌30min，得到均匀分散的陶瓷浆料；向陶瓷浆料中加入醋酸调节PH值为2，再将陶瓷浆料倒入模具中,并加入占陶瓷浆料0.6wt%的戊二醛作为引发剂于常温下静置经1.5小时固化成型后脱模，脱模后的样品在烘箱中于60℃烘干12小时, 再移入马弗炉中以5℃/min速率升温至1500℃，保温2h。得到的全晶须结构莫来石蜂窝陶瓷载体的孔隙率为77%，抗压强度为16MPa。
实施例4：向128ml水中加入300g陶瓷粉体，其中Al2O3、二氧化硅、氟化铝、五氧化二钒、三氧化钼质量比为65:25:4:3:3；并加入占粉体总质量0.5wt%的壳聚糖，将得到的混合物于常温下用磁力搅拌器搅拌30min，得到均匀分散的陶瓷浆料；向陶瓷浆料中加入醋酸调节PH值为2.5，再将陶瓷浆料倒入模具中,并加入占陶瓷浆料0.6wt%的戊二醛作为引发剂于常温下静置经3小时固化成型后脱模，脱模后的样品在烘箱中于60℃烘干12小时, 再移入马弗炉中以5℃/min速率升温至1500℃，保温2h；得到的全晶须结构莫来石蜂窝陶瓷载体的孔隙率为50%，抗压强度为80MPa。
实施例5：向300ml水中加入200g陶瓷粉体，其中Al2O3、二氧化硅、氟化铝质量比为78:21:1；并加入占粉体总质量0.5wt%的壳聚糖，将得到的混合物于常温下用磁力搅拌器搅拌30min，得到均匀分散的陶瓷浆料；向陶瓷浆料中加入醋酸调节PH值为5，再将陶瓷浆料倒入模具中,并加入占陶瓷浆料0.6wt%的戊二醛作为引发剂于常温下静置经5小时固化成型后脱模，脱模后的样品在烘箱中于60℃烘干12小时, 再移入马弗炉中以5℃/min速率升温至1500℃，保温2h；得到的全晶须结构莫来石蜂窝陶瓷载体的孔隙率为83%，抗压强度为5MPa。
Claims (5)
1.一种制备全晶须结构莫来石蜂窝陶瓷载体的方法，所述的制备方法以壳聚糖为有机聚合单体，戊二醛作为引发剂，氧化铝和二氧化硅作为莫来石前驱体粉末，外加晶须生长助剂，得到全部由莫来石晶须构成的蜂窝陶瓷块体材料，其具体步骤如下：
1）陶瓷浆料的制备：氧化铝、二氧化硅和晶须生长助剂按照65～78wt%：21～26wt% ：1～10wt%的重量比加入到水中，再加入占粉体总质量0.5 wt %的壳聚糖作为有机聚合单体配成固含量为40～70 wt %的陶瓷浆料，并在所述的陶瓷浆料中加入醋酸，使陶瓷浆料的PH值为1.5 ～5；
浆料的固化成型：将步骤1）所制备的陶瓷浆料倒入模具中并加入占陶瓷浆料总质量0.6%的戊二醛作为引发剂，然后在常温下静置0.5～5小时固化成型；
3）样品的烘干：将样品脱模后在40～80℃烘干5～20小时得到陶瓷坯体；
4）坯体的烧结：将步骤3）烘干得到的陶瓷坯体置于马弗炉中下以1～10℃/min升温至1000℃，保温0～3小时后，再以1～7℃/min 继续升温至1200～1600℃保温1～5小时使坯体烧结，然后随炉冷却，得到主晶相为莫来石相的全晶须结构莫来石蜂窝陶瓷载体。
2.如权利要求1所述的一种制备全晶须结构莫来石蜂窝陶瓷载体的方法，其特征在于：所述的晶须生长助剂为氟化铝、五氧化二钒、三氧化钼中的一种或几种的混合。
3.如权利要求1所述的一种制备全晶须结构莫来石蜂窝陶瓷载体的方法，其特征在于：所述的莫来石蜂窝陶瓷载体具有原位生长的晶须结构。
4.如权利要求1所述的一种制备全晶须结构莫来石蜂窝陶瓷载体的方法，其特征在于：所述莫来石蜂窝陶瓷的显气孔率为50%～83%。
5.如权利要求1所述的一种制备全晶须结构莫来石蜂窝陶瓷载体的方法，其特征在于：所述莫来石多孔陶瓷的抗压强度为5～80MPa。
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