CN107840677B - 一种氧化铝基泡沫陶瓷及其制备方法 - Google Patents
一种氧化铝基泡沫陶瓷及其制备方法 Download PDFInfo
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 97
- 239000000919 ceramic Substances 0.000 title claims abstract description 75
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Abstract
本发明涉及一种氧化铝基泡沫陶瓷及其制备方法，先将工业氧化铝、防爆纤维、辛醇、羧甲基纤维素、羟丙基甲基纤维素、聚羧酸盐和水混匀，制得浆体Ⅰ；将α‑氧化铝、辛醇、羧甲基纤维素、聚羧酸盐和水混匀，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，得到氧化铝基泡沫陶瓷预制体；然后用浆体Ⅱ对氧化铝基泡沫陶瓷预制体进行真空浸渍，压缩空气喷吹或者离心甩浆，自然干燥，得到氧化铝基泡沫陶瓷坯体，在一定条件下保温，制得氧化铝基泡沫陶瓷。本发明具有工艺简单、成本低特点，所制备的氧化铝基泡沫陶瓷机械强度高、热震稳定性好。
Description
技术领域
本发明涉及一种泡沫陶瓷技术领域，具体涉及一种氧化铝基泡沫陶瓷及其制备方法。
背景技术
采用有机泡沫浸渍法制备的泡沫陶瓷是以聚氨酯泡沫塑料作为前驱体，浸渍陶瓷浆体得到高孔隙率和三维网状结构的多孔材质。由于其结构的特殊性、耐腐蚀和良好的机械力学性能而被广泛的应用于航空航天、耐火材料、催化和过滤等领域。
氧化铝(Al2O3)具有高的机械强度、耐火度高、良好的抗侵蚀性、优异的介电性能和抗氧化性等一系列的优点。氧化铝泡沫陶瓷是一种重要的冶金过滤用耐火材料材料和建筑保温材料。但制备氧化铝基泡沫陶瓷时，由于聚氨酯模板在200～600℃分解产生中空三角形孔筋并且产生的挥发性气体导致陶瓷基体表面生成大量裂纹，影响了氧化铝基泡沫陶瓷的高温力学性能、热震稳定性和抗冲刷能力等。
“氧化铝质多孔泡沫陶瓷过滤器的制备方法”(CN201210500465)的专利技术，公开了一种以氧化铝微粉、铝矾土、滑石粉和膨润土组成陶瓷粉末，再加入粘结剂、分散剂和水制备浆料，以软质聚氨酯泡沫塑料为载体制备氧化铝质多孔泡沫陶瓷过滤器。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)并没有修饰由于聚氨酯泡沫塑料烧失后所产生的中空孔筋以及陶瓷基体表面的裂纹；(2)采用喷涂等工艺对生产设备要求较为复杂；(3)煅烧温度较低氧化铝并未烧结导致氧化铝泡沫陶瓷强度不高。
“一种复相氧化铝泡沫陶瓷材料及制备方法”(CN201310338211)的专利技术，公开了一种以氧化铝、碳化硅、硅微粉、高岭土、二氧化钛和滑石粉组成陶瓷粉末，再加入添加剂和水制备浆料，以预处理后的聚氨酯泡沫塑料为载体制备复相氧化铝泡沫陶瓷材料。该方法在一定程度上提升了复相氧化铝泡沫陶瓷的常温力学强度，降低了烧结温度。但其主要缺陷是：(1)加入烧结剂降低了氧化铝泡沫陶瓷的高温机械性能；(2)未修饰和由聚氨酯泡沫烧失而产生的缺陷，在受外界作用下易形成应力集中导致氧化铝泡沫陶瓷的损坏。
发明内容
本发明旨在克服现有技术缺陷，目的是提供一种氧化铝基泡沫陶瓷及其制备方法，用该方法制备的氧化铝基泡沫陶瓷强度高、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：
一种氧化铝基泡沫陶瓷，制备步骤如下：
步骤一、向100份质量的工业氧化铝中加入0.0005～0.0015份质量的防爆纤维、0.3～2.1份质量的辛醇、0.3～1.7份质量的羧甲基纤维素、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、向100份α-氧化铝中加入0.3～2.1份质量的辛醇、0.1～0.9份质量的羧甲基纤维素、0.3～1份质量的聚羧酸盐和28～55份质量的水，球磨1～1.5h，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1.5～2.5h，得到氧化铝基泡沫陶瓷预制体；然后将所述氧化铝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，得到氧化铝基泡沫陶瓷坯体；
步骤四、将所述的氧化铝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1550～1650℃，保温2～5h，在随炉冷却至室温，即得到氧化铝基泡沫陶瓷。
所述的工业氧化铝的平均粒度≤3μm。
所述的防爆纤维长度3～5mm，直径20μm。
所述的α-氧化铝平均粒径≤5μm。
与现有技术相比，本发明具有以下有益效果：
本发明先将工业氧化铝、防爆纤维、辛醇、羧甲基纤维素、羟丙基甲基纤维素、聚羧酸盐和水混匀，制得浆体Ⅰ；将α-氧化铝、辛醇、羧甲基纤维素、聚羧酸盐和水混匀，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1.5～2.5h，得到氧化铝基泡沫陶瓷预制体；然后用浆体Ⅱ对氧化铝基泡沫陶瓷预制体进行真空浸渍，压缩空气喷吹或者离心甩浆，自然干燥，得到氧化铝基泡沫陶瓷坯体；最后在空气气氛和1550～1650℃条件下保温2～5h，制得氧化铝基泡沫陶瓷。本发明具有工艺简单，成本低特点，所制备的氧化铝基泡沫陶瓷机械强度高、热震稳定性好。
本发明采用工业氧化铝和防爆纤维为主要原料制备浆料Ⅰ并涂覆至聚氨酯泡沫基体表面，600～850℃保温1.5～2.5h制备氧化铝基泡沫陶瓷预制体，由于防爆纤维的烧失和工业氧化铝在高温下相变所产生的微裂纹可使由聚氨酯泡沫分解产生的气体从中溢出，并且未对陶瓷基体产生明显的缺陷。
二次真空浸渍技术。通过二次真空浸渍技术将浆料Ⅱ涂覆至氧化铝基瓷预制体表面以及中空孔筋内部，可使氧化铝基筋因聚氨酯海绵挥发所产生的缺陷和中空孔筋得到修复，提高了氧化铝基泡沫陶瓷的机械性能和热震稳定性。
本发明制备的氧化铝基泡沫陶瓷，经检测：常温耐压强度为2.7～5.8MPa；1100℃水冷循环次数为12～25次；抗碱溶液冲刷侵蚀15～20h后试样的耐压强度为2.3～5.7MPa。
因此，本发明制备的氧化铝基泡沫陶瓷的强度高、热震稳定性好，具有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：
所述的工业氧化铝的平均粒度≤3μm；
所述的防爆纤维长度3～5mm，直径20μm；
所述的α-氧化铝平均粒径≤5μm。
实施例1
步骤一、向100份质量的工业氧化铝中加入0.0005～0.0008份质量的防爆纤维、0.3～2.1份质量的辛醇、0.3～1.7份质量的羧甲基纤维素、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、向100份α-氧化铝中加入0.3～1.5份质量的辛醇、0.1～0.5份质量的羧甲基纤维素、0.3～1份质量的聚羧酸盐和28～40份质量的水，球磨1～1.5h，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1.5～2.5h，得到氧化铝基泡沫陶瓷预制体；然后将所述氧化铝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，得到氧化铝基泡沫陶瓷坯体。
步骤四、将所述的氧化铝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1550～1600℃，保温2～5h，在随炉冷却至室温，即得到氧化铝基泡沫陶瓷。
本实施例1所制备的氧化铝基泡沫陶瓷，经检测：常温耐压强度为2.7～4.1MPa；1100℃水冷循环次数为17～23次；抗碱溶液冲刷侵蚀15～20h后试样的耐压强度为2.3～3.9MPa。
实施例2
一种氧化铝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、向100份α-氧化铝中加入1.5～2.1份质量的辛醇、0.5～0.9份质量的羧甲基纤维素、0.3～1份质量的聚羧酸盐和40～55份质量的水，球磨1～1.5h，制得浆体Ⅱ；
本实施例2所制备的氧化铝基泡沫陶瓷，经检测：常温耐压强度为3.1～4.7MPa；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3.0～4.5MPa。
实施例3
步骤一、向100份质量的工业氧化铝中加入0.0008～0.0015份质量的防爆纤维、0.3～2.1份质量的辛醇、0.3～1.7份质量的羧甲基纤维素、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、向100份α-氧化铝中加入0.3～1.5份质量的辛醇、0.1～0.5份质量的羧甲基纤维素、0.3～1份质量的聚羧酸盐和28～40份质量的水，球磨1～1.5h，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1.5～2.5h，得到氧化铝基泡沫陶瓷预制体；然后将所述氧化铝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，得到氧化铝基泡沫陶瓷坯体。
步骤四、将所述的氧化铝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1600～1650℃，保温2～5h，在随炉冷却至室温，即得到氧化铝基泡沫陶瓷。
本实施例3所制备的氧化铝基泡沫陶瓷，经检测：常温耐压强度为4.5～5.2MPa；1100℃水冷循环次数为12～18次；抗碱溶液冲刷侵蚀15～20h后试样的耐压强度为4.3～5.1MPa。
实施例4
一种氧化铝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、向100份质量的α-氧化铝中加入1.5～2.1份质量的辛醇、0.5～0.9份质量的羧甲基纤维素、0.3～1份质量的聚羧酸盐和40～55份质量的水，球磨1～1.5h，制得浆体Ⅱ；
本实施例4所制备的氧化铝基泡沫陶瓷，经检测：常温耐压强度为4.7～5.8MPa；1100℃水冷循环次数为15～20次；抗碱溶液冲刷侵蚀15～20h后试样的耐压强度为4.5～5.7MPa。
本发明采用工业氧化铝和防爆纤维为主要原料制备浆料Ⅰ并涂覆至聚氨酯泡沫基体表面，600～850℃保温1.5～2.5h制备氧化铝基泡沫陶瓷预制体，由于防爆纤维的烧失和工业氧化铝在高温下相变所产生的微裂纹可使由聚氨酯泡沫分解产生的气体从中溢出，并且未对陶瓷基体产生明显的缺陷。
二次真空浸渍技术。通过二次真空浸渍技术将浆料Ⅱ涂覆至氧化铝基瓷预制体表面以及中空孔筋内部，可使氧化铝基筋因聚氨酯海绵挥发所产生的缺陷和中空孔筋得到修复，提高了氧化铝基泡沫陶瓷的机械性能和热震稳定性。
本发明制备的氧化铝基泡沫陶瓷，经检测：常温耐压强度为2.7～5.8MPa；水冷循环次数为12～25次；抗碱溶液冲刷侵蚀15～20h后试样的耐压强度为2.3～5.7MPa。
因此，本发明制备的氧化铝基泡沫陶瓷的强度高、热震稳定性好，具有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)
1.一种氧化铝基泡沫陶瓷，其特征在于：制备步骤如下：
步骤一、向100份质量的工业氧化铝中加入0.0005~0.0015份质量的防爆纤维、0.3~2.1份质量的辛醇、0.3~1.7份质量的羧甲基纤维素、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、向100份质量的α-氧化铝中加入0.3~2.1份质量的辛醇、0.1~0.9份质量的羧甲基纤维素、0.3~1份质量的聚羧酸盐和28~55份质量的水，球磨1~1.5h，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1.5~2.5h，得到氧化铝基泡沫陶瓷预制体；然后将所述氧化铝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，得到氧化铝基泡沫陶瓷坯体；
步骤四、将所述的氧化铝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1550~1650℃，保温2~5h，在随炉冷却至室温，即得到氧化铝基泡沫陶瓷。
2.根据权利要求1所述的氧化铝基泡沫陶瓷，其特征在于： 所述的工业氧化铝的平均粒度≤3μm。
3.根据权利要求1所述的氧化铝基泡沫陶瓷，其特征在于：所述的防爆纤维长度3~5mm，直径20μm。
4.根据权利要求1所述的氧化铝基泡沫陶瓷，其特征在于：所述的α-氧化铝平均粒径≤5μm。
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