CN107698246B - 一种多层骨架结构的刚玉-莫来石基泡沫陶瓷及其制备方法 - Google Patents
一种多层骨架结构的刚玉-莫来石基泡沫陶瓷及其制备方法 Download PDFInfo
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Abstract
本发明涉及一种多层骨架结构的刚玉‑莫来石基泡沫陶瓷及其制备方法,先将氧化铝微粉和硅微粉、聚甲基丙烯酸铵、羟丙基甲基纤维素、聚羧酸盐和水混匀,制得浆体Ⅰ;将氧化铝微粉、硅源和硅溶胶混匀,制得浆体Ⅱ;再在真空条件下将聚氨酯海绵浸渍于浆体Ⅰ中,采用压缩空气喷吹或者离心甩浆,自然干燥,保温,得到刚玉‑莫来石基泡沫陶瓷预制体;然后用浆体Ⅱ对刚玉‑莫来石基泡沫陶瓷预制体坯进行真空浸渍,压缩空气喷吹或者离心甩浆,自然干燥;最后在一定条件下保温,即得多层骨架结构刚玉‑莫来石基泡沫陶瓷。本发明制备的多层骨架结构的刚玉‑莫来石基泡沫陶瓷的强度高、热震稳定性好和优异的抗侵蚀冲刷能力。
Description
技术领域
本发明属于泡沫陶瓷技术领域,具体涉及一种多层骨架结构的刚玉-莫来石基泡沫陶瓷及其制备方法。
背景技术
泡沫陶瓷是具有三维空间网架构的高气孔率的多孔陶瓷体。由于它具有高气孔率、比表面积大、机械强度高、耐高温和化学腐蚀等性能而被广泛的应用于热交换材料、净化冶金工业过滤熔融金属、工业废气和废水的处理以及化学催化剂载体等。但是,采用有机泡沫浸渍法制备的刚玉-莫来石基泡沫陶瓷由于聚氨酯基体在200~600℃分解原位产生中空的孔筋以及所产生的挥发性气体导致陶瓷基体表面生成大量的缺陷,致使刚玉-莫来石基泡沫陶瓷的机械强度和热震稳定性显著降低。
莫来石(3Al2O3·2SiO2)是Al2O3-SiO2二元系统中常压下唯一稳定的二元固溶体,其拥有耐高温(熔点为1850℃)、机械强度高和导热系数小等优异的性能。刚玉(α-Al2O3)作为氧化铝中最稳定相其晶体结构中O作六方最紧密堆积,Al填充在2/3的O八面体孔隙中,从而使化学式为Al2O3。刚玉中Al和O做紧密堆积并且晶体中Al-O正负离子间化学键强,晶格能较大,使得其具有抗侵蚀、高熔点、机械强度高、耐磨性好等优良性能而被广泛的应用工业领域。结合刚玉和莫来石的优良性能所制备的刚玉-莫来石基泡沫具有较好的机械强度和良好的体积稳定性。
但是,目前技术人员为进一步优化和提升泡沫陶瓷的力学性能和热震稳定性等问题进行了深入的研究和技术开发:
“氧化锆质泡沫陶瓷过滤器”(ZL200710139288)的专利技术,公开了一种以氧化锆、氧化铝、氧化钙、氧化钇组成陶瓷粉末,再加入甲基纤维素、聚乙烯醇和水制备浆料,以软质聚氨酯泡沫塑料为载体制备氧化锆质泡沫陶瓷过滤器。该方法在一定程度上提升了氧化锆泡沫陶瓷过滤器的耐高温和耐热冲击性能。但其主要缺陷是:(1)为改善净化金属熔液的能力;(2)未加消泡剂;(3)聚氨酯泡沫塑料烧失后产生的中空孔筋,易产生应力集中,降低材料的力学性能。
“一种制备SiC泡沫陶瓷过滤器的方法”(ZL201110371525)的专利技术,公开了一种以碳化硅粉、氧化铝粉、锂基膨润土组成陶瓷粉末,再加入粘结剂和水制备浆料,以预处理后的聚氨酯泡沫塑料为载体制备SiC泡沫陶瓷。该方法在一定程度上提升了SiC的常温机械性能。但其主要缺陷是:(1)未对聚氨酯泡沫塑料原位分解产生的中空孔筋进行处理,在受外界应力作用下易形成应力集中致使泡沫陶瓷损坏;(2)采用该技术制备的SiC泡沫陶瓷中含有玻璃相降低了泡沫陶瓷的热震稳定性和高温力学性能。
发明内容
本发明旨在克服现有技术缺陷,目的是提供一种多层骨架结构的刚玉-莫来石基泡沫陶瓷及其制备方法,用该方法制备的多层骨架结构的刚玉-莫来石基泡沫陶瓷强度高、抗热震性能好。
为实现上述发明目的,本发明提供的技术方案是:
一种多层骨架结构的刚玉-莫来石基泡沫陶瓷,制备步骤如下:
步骤一、将60~80份质量的氧化铝微粉与20~40份质量的硅微粉混合,得混合粉Ⅰ;再向混合粉Ⅰ中加入0.3~2.1份质量的聚甲基丙烯酸铵、0.2~1.1份质量的羟丙基甲基纤维素、0.3~1份质量的聚羧酸盐和22~49份质量的水,球磨1~1.5h,制得浆体Ⅰ;
步骤二、将72~90份质量的氧化铝微粉中加入10~28份质量的硅源混合,得混合粉Ⅱ;再向混合粉Ⅱ中加入27~50份质量的硅溶胶,机械球磨1~3h,制得浆体Ⅱ;
步骤三、将聚氨酯海绵在真空条件下浸入浆体Ⅰ中,浸渍后压缩空气喷吹或者离心甩浆,经自然干燥12~24h,再以0.5~2℃/min的速率升温至600~850℃,保温0.5~1.5h,得到刚玉-莫来石基泡沫陶瓷预制体;然后将所述刚玉-莫来石基泡沫陶瓷预制体在真空条件下浸入浆体Ⅱ中,浸渍后压缩空气喷出或者离心甩浆,自然干燥,得到刚玉-莫来石基泡沫陶瓷坯体;
步骤四、将所述的刚玉-莫来石基泡沫陶瓷坯体置入高温炉内,于空气气氛下,以2~3℃/min的速度升至1350~1550℃,保温2~5h,在随炉冷却至室温,即得到多层骨架结构的刚玉-莫来石基泡沫陶瓷。
所述的氧化铝的平均粒度≤7μm。
所述的硅溶胶浓度为1~3wt%。
所述的硅源为蓝晶石、红柱石、硅线石中的一种或多种的混合,平均粒径≤25μm。
与现有技术相比,本发明具有以下有益效果:
本发明先将氧化铝微粉和硅微粉、聚甲基丙烯酸铵、羟丙基甲基纤维素、聚羧酸盐和水混匀,制得浆体Ⅰ;将氧化铝微粉、硅源和硅溶胶混匀,制得浆体Ⅱ。再在真空条件下将聚氨酯海绵浸渍于浆体Ⅰ中,采用压缩空气喷吹或者离心甩浆,自然干燥12~24h,600~850℃保温0.5~1.5h,得到刚玉-莫来石基泡沫陶瓷预制体;然后用浆体Ⅱ对刚玉-莫来石基泡沫陶瓷预制体坯进行真空浸渍,压缩空气喷吹或者离心甩浆,自然干燥,;最后在空气气氛和1350~1550℃条件下保温2~5h,即得多层骨架结构刚玉-莫来石基泡沫陶瓷。本发明所制备的多层骨架结构的刚玉-莫来石基泡沫陶瓷是基于高温空气气氛条件下的原位反应烧结,不涉及特殊的喷涂工艺和保护气氛,故工艺简单和成本较低。
本发明采用二次真空浸渍技术,通过二次真空浸渍技术将浆料Ⅱ涂覆至刚玉-莫来石基陶瓷预制体表面以及中空孔筋内部,可使刚玉-莫来石孔筋因聚氨酯海绵挥发所产生的缺陷和中空孔筋得到修复,提高了刚玉-莫来石基泡沫陶瓷的机械性能和热震稳定性。
浆料Ⅱ中的硅源选用蓝晶石、硅线石和红柱石可在高温条件下发生分解反应生成莫来石和二氧化硅产生体积膨胀,并且在高温条件下蓝晶石、硅线石和红柱石分解所产生的二氧化硅与氧化铝微粉发生二次莫来石化产生体积膨胀,填充了由聚氨酯挥发原位生成的中空孔筋,并且在基体中形成微小裂纹,提升刚玉-莫来石基泡沫陶瓷的高温力学性能和热震稳定性。
本发明制备的多层骨架结构的刚玉-莫来石基泡沫陶瓷,经检测:常温耐压强度为2.5~5.5MPa;水冷循环次数为20~30次;抗碱溶液冲刷侵蚀15~20h后试样的耐压强度为2.25~5.3MPa。
因此,本发明制备的多层骨架结构的刚玉-莫来石基泡沫陶瓷的强度高、热震稳定性好和优异的抗侵蚀冲刷能力。
具体实施方式
下面结合具体实施例对本发明作进一步说明。
为避免重复,先将本具体实施方式所要涉及的技术参数统一描述如下,实施例中将不赘述:
所述的氧化铝微粉的平均粒度≤7μm;
所述的蓝晶石、红柱石和硅线石平均粒径≤25μm。
实施例1
步骤一、将60~70份质量的氧化铝微粉与30~40份质量的硅微粉混合,得混合粉Ⅰ;再向混合粉Ⅰ中加入0.3~1.1份质量的聚甲基丙烯酸铵、0.2~0.8份质量的羟丙基甲基纤维素、0.3~0.5份质量的聚羧酸盐和22~49份质量的水,球磨1~1.5h,制得浆体Ⅰ;
步骤二、将81~90份质量的氧化铝微粉中加入10~19份质量的蓝晶石混合,得混合粉Ⅱ;再向混合粉Ⅱ中加入27~50份质量浓度为1~2wt%的硅溶胶,机械球磨1~3h,制得浆体Ⅱ。
步骤三、将聚氨酯海绵在真空条件下浸入浆体Ⅰ中,浸渍后压缩空气喷吹或者离心甩浆,经自然干燥12~24h,再以0.5~2℃/min的速率升温至600~850℃,保温0.5~1.5h,得到刚玉-莫来石基泡沫陶瓷预制体;然后将所述刚玉-莫来石基泡沫陶瓷预制体在真空条件下浸入浆体Ⅱ中,浸渍后压缩空气喷出或者离心甩浆,自然干燥,得到刚玉-莫来石基泡沫陶瓷坯体。
步骤四、将所述的刚玉-莫来石基泡沫陶瓷坯体置入高温炉内,于空气气氛下,以2~3℃/min的速度升至1350~1450℃,保温2~5h,在随炉冷却至室温,即得到多层骨架结构的刚玉-莫来石基泡沫陶瓷。
本实施例1所制备的多层骨架结构的刚玉-莫来石基泡沫陶瓷,经检测:常温耐压强度为2.5~3.7MPa;1100℃水冷循环次数为21~23次;抗碱溶液冲刷侵蚀15~20h后试样的耐压强度为2.25~3.6MPa。
实施例2
一种多层骨架结构的刚玉-莫来石基泡沫陶瓷及其制备方法。本实施例所示制备方法除步骤二外,其余同实施例1。
步骤二、将72~81份氧化铝微粉中加入19~28份质量的红柱石混合,得混合粉Ⅱ;再向混合粉Ⅱ中加入27~50份质量浓度为2~3wt%硅溶胶,机械球磨1~3h,制得浆体Ⅱ。
本实施例2所制备的多层骨架结构的刚玉-莫来石基泡沫陶瓷,经检测:常温耐压强度为2.7~3.5MPa;1100℃水冷循环次数为22~25次;抗碱溶液冲刷侵蚀15~20h后试样的耐压强度为2.5~3.5MPa。
实施例3
步骤一、将70~80份质量的氧化铝微粉与20~30份质量的硅微粉混合,得混合粉Ⅰ;再向混合粉Ⅰ中加入0.3~1.1份质量的聚甲基丙烯酸铵、0.2~0.8份质量的羟丙基甲基纤维素、0.3~0.5份质量的聚羧酸盐和22~49份质量的水,球磨1~1.5h,制得浆体Ⅰ;
步骤二、将81~90份质量的氧化铝微粉中加入10~19份质量的硅线石混合,得混合粉Ⅱ;再向混合粉Ⅱ中加入27~50份质量浓度为1~2wt%的硅溶胶,机械球磨1~3h,制得浆体Ⅱ。
步骤三、将聚氨酯海绵在真空条件下浸入浆体Ⅰ中,浸渍后压缩空气喷吹或者离心甩浆,经自然干燥12~24h,再以0.5~2℃/min的速率升温至600~850℃,保温0.5~1.5h,得到刚玉-莫来石基泡沫陶瓷预制体;然后将所述刚玉-莫来石基泡沫陶瓷预制体在真空条件下浸入浆体Ⅱ中,浸渍后压缩空气喷出或者离心甩浆,自然干燥,得到刚玉-莫来石基泡沫陶瓷坯体。
步骤四、将所述的刚玉-莫来石基泡沫陶瓷坯体置入高温炉内,于空气气氛下,以2~3℃/min的速度升至1450~1550℃,保温2~5h,在随炉冷却至室温,即得到多层骨架结构的刚玉-莫来石基泡沫陶瓷。
本实施例3所制备的多层骨架结构的刚玉-莫来石基泡沫陶瓷,经检测:常温耐压强度为4.5~5.5MPa;1100℃水冷循环次数为25~29次;抗碱溶液冲刷侵蚀15~20h后试样的耐压强度为4.3~5.15MPa。
实施例4
一种多层骨架结构的刚玉-莫来石基泡沫陶瓷及其制备方法。本实施例所示制备方法除步骤二外,其余同实施例3。
步骤二、将72~81份质量的氧化铝微粉中加入8~10份质量的蓝晶石、5~7份质量的硅线石和6~11份质量的红柱石混合,得混合粉Ⅱ;再向混合粉Ⅱ中加入27~50份质量浓度为2~3wt%的硅溶胶,机械球磨1~3h,制得浆体Ⅱ。
本实施例4所制备的多层骨架结构的刚玉-莫来石基泡沫陶瓷,经检测:常温耐压强度为4.7~5.5MPa;1100℃水冷循环次数为26~30次;抗碱溶液冲刷侵蚀15~20h后试样的耐压强度为4.5~5.3MPa。
本发明采用二次真空浸渍技术。通过二次真空浸渍技术将浆料Ⅱ涂覆至刚玉-莫来石陶瓷预制体表面以及中空孔筋内部,可使刚玉-莫来石孔筋因聚氨酯海绵挥发所产生的缺陷和中空孔筋得到修复,提高了刚玉-莫来石泡沫陶瓷的机械性能和热震稳定性。
浆料Ⅱ中的硅源选用蓝晶石、硅线石和红柱石可在高温条件下发生分解反应生成莫来石和二氧化硅产生体积膨胀,并且在高温条件下蓝晶石、硅线石和红柱石分解所产生的二氧化硅与氧化铝微粉发生二次莫来石化产生体积膨胀,填充了由聚氨酯挥发原位生成的中空孔筋,并且在基体中形成微小裂纹,提升刚玉-莫来石基泡沫陶瓷的高温力学性能和热震稳定性。
本发明制备的多层骨架结构的刚玉-莫来石基泡沫陶瓷,经检测:常温耐压强度为2.5~5.5MPa;水冷循环次数为20~30次;抗碱溶液冲刷侵蚀15~20h后试样的耐压强度为2.25~5.3MPa。
因此,本发明制备的多层骨架结构的刚玉-莫来石基泡沫陶瓷的强度高、热震稳定性好和优异的抗侵蚀冲刷能力。
以上所述,仅是本发明的较佳实施例,并非对本发明作任何形式上的限制,任何熟悉本专业的技术人员,在不脱离本发明技术方案范围内,依据本发明的技术实质,对以上实施例所作的任何简单的修改、等同替换与改进等,均仍属于本发明技术方案的保护范围之内。
Claims (4)
1.一种多层骨架结构的刚玉-莫来石基泡沫陶瓷,其特征在于:制备步骤如下:
步骤一、将70~80份质量的氧化铝微粉与20~30份质量的硅微粉混合,得混合粉Ⅰ;再向混合粉Ⅰ中加入0.3~1.1份质量的聚甲基丙烯酸铵、0.2~0.8份质量的羟丙基甲基纤维素、0.3~0.5份质量的聚羧酸盐和22~49份质量的水,球磨1~1.5h,制得浆体Ⅰ;
步骤二、将72~81份质量的氧化铝微粉中加入8~10份质量的蓝晶石、5~7份质量的硅线石和6~11份质量的红柱石混合,得混合粉Ⅱ;再向混合粉Ⅱ中加入27~50份质量浓度为2~3wt%的硅溶胶,机械球磨1~3h,制得浆体Ⅱ;
步骤三、将聚氨酯海绵在真空条件下浸入浆体Ⅰ中,浸渍后压缩空气喷吹或者离心甩浆,经自然干燥12~24h,再以0.5~2℃/min的速率升温至600~850℃,保温0.5~1.5h,得到刚玉-莫来石基泡沫陶瓷预制体;然后将所述刚玉-莫来石基泡沫陶瓷预制体在真空条件下浸入浆体Ⅱ中,浸渍后压缩空气喷出或者离心甩浆,自然干燥,得到刚玉-莫来石基泡沫陶瓷坯体;
步骤四、将所述的刚玉-莫来石基泡沫陶瓷坯体置入高温炉内,于空气气氛下,以2~3℃/min的速度升至1450~1550℃,保温2~5h,再随炉冷却至室温,即得到多层骨架结构的刚玉-莫来石基泡沫陶瓷。
2.根据权利要求1所述的多层骨架结构的刚玉-莫来石基泡沫陶瓷,其特征在于:所述的氧化铝的平均粒度≤7μm。
3.根据权利要求1所述的多层骨架结构的刚玉-莫来石基泡沫陶瓷,其特征在于:所述的硅溶胶浓度为1~3wt%。
4.根据权利要求1所述的多层骨架结构的刚玉-莫来石基泡沫陶瓷,其特征在于:所述的蓝晶石、硅线石和红柱石的平均粒径≤25μm。
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