CN111978074A - 一种碳纳米管增强的多孔陶瓷型芯及其制备方法 - Google Patents

一种碳纳米管增强的多孔陶瓷型芯及其制备方法 Download PDF

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CN111978074A
CN111978074A CN202010757889.3A CN202010757889A CN111978074A CN 111978074 A CN111978074 A CN 111978074A CN 202010757889 A CN202010757889 A CN 202010757889A CN 111978074 A CN111978074 A CN 111978074A
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杨玮
梁书锦
王庆相
赖运金
张鹏
刘海浪
杨文广
康路
黄椿森
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Xi'an Sino Euro Materials Technologies Co ltd
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Abstract

本发明公开了一种碳纳米管增强的多孔陶瓷型芯，按照质量百分比由以下成分组成：基体Al2O3粉末65％～79％，矿化剂MgO粉末2％～6％，成孔剂8％～12％，增塑剂10％～15％，碳纳米管1％～2％。本发明还公开了一种碳纳米管增强的多孔陶瓷型芯的制备方法。

Description

一种碳纳米管增强的多孔陶瓷型芯及其制备方法
技术领域
本发明属于陶瓷制备技术领域，具体涉及一种碳纳米管增强的多孔陶瓷型芯，还涉及一种碳纳米管增强的多孔陶瓷型芯的制备方法。
背景技术
陶瓷型芯是制造高性能涡轮叶片的关键部件，与氧化硅基陶瓷型芯相比，氧化铝基陶瓷型芯具有熔点高2054℃、化学稳定性能和抗蠕变性能好等优点，可形成具有高尺寸精度的叶片内腔，提高叶片的合格率。但是氧化铝基陶瓷型芯的α-Al2O3化学性能稳定，常温常压下很难与酸碱腐蚀液发生反应，脱出性较差，成为制约氧化铝基陶瓷型芯广泛使用的一大瓶颈。
型芯气孔率是反映型芯脱芯性能好坏的重要指标之一，开展氧化铝基陶瓷型芯内部气孔率的研究，对解决其脱除困难的问题，具有十分重要的意义。成孔剂可以有效的增加型芯的气孔率。淀粉价格便宜，无毒易得，容易烧失，是一种较为理想的成孔剂。研究发现虽然加入成孔剂淀粉会获得多孔氧化铝基陶瓷型芯，但是陶瓷型芯的致密度降低，强度显著下降。
直管型单壁碳纳米管由于其优异的力学性能和高的导热性能、优异的机械稳定性和化学稳定性、良好的溶液加工性和高柔性。由于碳纳米管中碳原子采取SP2杂化，相比SP3杂化，SP2杂化中S轨道成分比较大，使碳纳米管具有高模量和高强度。碳纳米管具有良好的力学性能，抗拉强度达到50～200GPa，是钢的100倍，密度却只有钢的1/6，至少比常规石墨纤维高一个数量级；它的弹性模量可达1TPa，与金刚石的弹性模量相当，约为钢的5倍。对于具有理想结构的单层壁的碳纳米管，其抗拉强度约800GPa。碳纳米管是目前可制备出的具有最高比强度的材料。若将以其他工程材料为基体与碳纳米管制成复合材料，可使复合材料表现出良好的强度、弹性、抗疲劳性及各向同性，给复合材料的性能带来极大的改善。因此在多孔陶瓷型芯中加入碳纳米管，可以获得具有良好力学性能的高气孔率氧化铝基陶瓷型芯。
发明内容
本发明的第一个目的是提供一种碳纳米管增强的多孔陶瓷型芯，解决现有多孔陶瓷型芯存在力学性能较差的问题。
为了达到上述目的，本发明所采用的技术方案是：一种碳纳米管增强的多孔陶瓷型芯，按照质量百分比由以下成分组成：
基体Al2O3粉末65％～79％，矿化剂MgO粉末2％～6％，成孔剂8％～12％，增塑剂10％～15％，碳纳米管1％～2％。
本发明的技术方案，还具有以下特点：
所述成孔剂为淀粉。
所述增塑剂为石蜡。
所述Al2O3粉末粒度为180目的占60％-65％，粒度为280目的占35％-40％。
所述MgO粉末的粒度为240目。
所述碳纳米管属于直管型单壁碳纳米管，碳纳米管的长度直径比大于25:1。
本发明的第二个目的是提供一种碳纳米管增强的多孔陶瓷型芯的制备方法，解决现有多孔陶瓷型芯存在力学性能较差的问题。
为了达到上述目的，本发明所采用的技术方案是：一种碳纳米管增强的多孔陶瓷型芯的制备方法，具体按照以下步骤实施：
步骤1，各成分按照对应质量比称取，先将增塑剂石蜡加热到60℃～70℃，再按照上述比例加入Al2O3粉末、MgO粉末、淀粉和碳纳米管并不断搅拌，搅拌时间3h-4h，得到混合均匀的浆料；
步骤2，将混合均匀的浆料加入到热压注机，制备陶瓷型芯坯体；
步骤3，将制得的陶瓷型芯坯体冷冻干燥，温度-46～-50℃，时间5h；
步骤4，将步骤3得到的陶瓷型芯坯体埋在氧化铝的刚玉匣钵中，进行烧结，得到目标碳纳米管增强的多孔陶瓷型芯。
本发明的技术方案，还具有以下特点：
在所述步骤2中，热压注机模具预热温度50℃～60℃，注射压力12Mpa～15Mpa，压注时间15s～17s。
在所述步骤3中，冷冻干燥的为温度-46～-50℃，时间为5h。
在所述步骤4中，烧结具体为：先室温升至420℃～450℃，升温速率4℃/min～5℃/min，保温时间2h；之后升温至900℃～920℃，升温速率8℃/min～10℃/min，保温时间1h；再升温至1770℃～1780℃，升温速率8℃/min～10℃/min，保温时间3h，然后断电，随炉冷却。
与现有技术相比，本发明的制备方法制备得到的碳纳米管增强的多孔陶瓷型芯，在加入成孔剂淀粉的陶瓷型芯中加入了适量的碳纳米管，再进行高温烧结获得气孔率30％～75％，陶瓷型芯的室温抗弯强度为35MPa～70MPa，在1650℃的高温下抗弯强度为25MPa～45MPa，同时表现出良好的抗冲击性能和溶出性，解决了多孔陶瓷型芯的力学性能较差的特性，有利于制备高强度，易脱除的陶瓷型芯。
具体实施方式
以下结合具体实施例对本发明的技术方案作进一步地详细说明。
本发明的一种碳纳米管增强的多孔陶瓷型芯，按照质量百分比由以下成分组成：
基体Al2O3粉末65％～79％，矿化剂MgO粉末2％～6％，成孔剂淀粉8％～12％，增塑剂石蜡10％～15％，碳纳米管1％～2％；其中：Al2O3粉末粒度为180目的占60％-65％，粒度为280目的占35％-40％，MgO粉末的粒度为240目；碳纳米管属于直管型单壁碳纳米管，碳纳米管的长度直径比大于25:1。
本发明的上述碳纳米管增强的多孔陶瓷型芯的制备方法，具体按照以下步骤实施：
步骤1，各成分按照对应质量比称取，先将增塑剂石蜡加热到60℃～70℃，再按照上述比例加入Al2O3粉末、MgO粉末、淀粉和碳纳米管并不断搅拌，搅拌时间3h-4h，得到混合均匀的浆料；
步骤2，将混合均匀的浆料加入到热压注机，制备陶瓷型芯坯体；热压注机模具预热温度50℃～60℃，注射压力12Mpa～15Mpa，压注时间15s～17s
步骤3，将制得的陶瓷型芯坯体冷冻干燥，冷冻干燥的为温度-46～-50℃，时间为5h；
步骤4，将步骤3得到的陶瓷型芯坯体埋在氧化铝的刚玉匣钵中，进行烧结，得到目标碳纳米管增强的多孔陶瓷型芯；烧结具体为：先室温升至420℃～450℃，升温速率4℃/min～5℃/min，保温时间2h；之后升温至900℃～920℃，升温速率8℃/min～10℃/min，保温时间1h；再升温至1770℃～1780℃，升温速率8℃/min～10℃/min，保温时间3h，然后断电，随炉冷却。
本发明的制备方法制备得到的碳纳米管增强的多孔陶瓷型芯，在加入成孔剂淀粉的陶瓷型芯中加入了适量的碳纳米管，再进行高温烧结获得气孔率30％～75％，陶瓷型芯的室温抗弯强度为35MPa～70MPa，在1650℃的高温下抗弯强度为25MPa～45MPa，同时表现出良好的抗冲击性能和溶出性，解决了多孔陶瓷型芯的力学性能较差的特性，有利于制备高强度，易脱除的陶瓷型芯。
实施例1
本发明的一种碳纳米管增强的多孔陶瓷型芯，按照质量百分比由以下成分组成：
基体Al2O3粉末65％，矿化剂MgO粉末6％，成孔剂淀粉12％，增塑剂石蜡15％，碳纳米管2％；其中：Al2O3粉末粒度为180目的占60％，粒度为280目的占40％，MgO粉末的粒度为240目；碳纳米管属于直管型单壁碳纳米管，碳纳米管的长度直径比为26:1。
本发明的上述碳纳米管增强的多孔陶瓷型芯的制备方法，具体按照以下步骤实施：
步骤1，各成分按照对应质量比称取，先将增塑剂石蜡加热到60℃，再按照上述比例加入Al2O3粉末、MgO粉末、淀粉和碳纳米管并不断搅拌，搅拌时间3h，得到混合均匀的浆料；
步骤2，将混合均匀的浆料加入到热压注机，制备陶瓷型芯坯体；热压注机模具预热温度50℃，注射压力12Mpa，压注时间15s；
步骤3，将制得的陶瓷型芯坯体冷冻干燥，冷冻干燥的为温度-46，时间为5h；
步骤4，将步骤3得到的陶瓷型芯坯体埋在氧化铝的刚玉匣钵中，进行烧结，得到目标碳纳米管增强的多孔陶瓷型芯；烧结具体为：先室温升至420℃，升温速率4℃/min，保温时间2h；之后升温至900℃，升温速率8℃/min，保温时间1h；再升温至1770℃，升温速率8℃/min，保温时间3h，然后断电，随炉冷却。
实施例2
本发明的一种碳纳米管增强的多孔陶瓷型芯，按照质量百分比由以下成分组成：
基体Al2O3粉末72％，矿化剂MgO粉末4％，成孔剂淀粉10％，增塑剂石蜡12.5％，碳纳米管1.5％；其中：Al2O3粉末粒度为180目的占62.5％，粒度为280目的占37.5％，MgO粉末的粒度为240目；碳纳米管属于直管型单壁碳纳米管，碳纳米管的长度直径比大于28:1。
本发明的上述碳纳米管增强的多孔陶瓷型芯的制备方法，具体按照以下步骤实施：
步骤1，各成分按照对应质量比称取，先将增塑剂石蜡加热到65℃，再按照上述比例加入Al2O3粉末、MgO粉末、淀粉和碳纳米管并不断搅拌，搅拌时间3.5h，得到混合均匀的浆料；
步骤2，将混合均匀的浆料加入到热压注机，制备陶瓷型芯坯体；热压注机模具预热温度55℃，注射压力13.5Mpa，压注时间16s；
步骤3，将制得的陶瓷型芯坯体冷冻干燥，冷冻干燥的为温度-48℃，时间为5h；
步骤4，将步骤3得到的陶瓷型芯坯体埋在氧化铝的刚玉匣钵中，进行烧结，得到目标碳纳米管增强的多孔陶瓷型芯；烧结具体为：先室温升至435℃，升温速率4.5℃/min，保温时间2h；之后升温至910℃，升温速率9℃/min，保温时间1h；再升温至1775℃，升温速率9℃/min，保温时间3h，然后断电，随炉冷却。
实施例3
本发明的一种碳纳米管增强的多孔陶瓷型芯，按照质量百分比由以下成分组成：
基体Al2O3粉末79％，矿化剂MgO粉末2％，成孔剂淀粉8％，增塑剂石蜡10％，碳纳米管1％；其中：Al2O3粉末粒度为180目的占65％，粒度为280目的占35％，MgO粉末的粒度为240目；碳纳米管属于直管型单壁碳纳米管，碳纳米管的长度直径比大于29:1。
本发明的上述碳纳米管增强的多孔陶瓷型芯的制备方法，具体按照以下步骤实施：
步骤1，各成分按照对应质量比称取，先将增塑剂石蜡加热到70℃，再按照上述比例加入Al2O3粉末、MgO粉末、淀粉和碳纳米管并不断搅拌，搅拌时间4h，得到混合均匀的浆料；
步骤2，将混合均匀的浆料加入到热压注机，制备陶瓷型芯坯体；热压注机模具预热温度60℃，注射压力15Mpa，压注时间17s；
步骤3，将制得的陶瓷型芯坯体冷冻干燥，冷冻干燥的为温度-50℃，时间为5h；
步骤4，将步骤3得到的陶瓷型芯坯体埋在氧化铝的刚玉匣钵中，进行烧结，得到目标碳纳米管增强的多孔陶瓷型芯；烧结具体为：先室温升至450℃，升温速率5℃/min，保温时间2h；之后升温至920℃，升温速率10℃/min，保温时间1h；再升温至1780℃，升温速率10℃/min，保温时间3h，然后断电，随炉冷却。

Claims (10)

1.一种碳纳米管增强的多孔陶瓷型芯，其特征在于，按照质量百分比由以下成分组成：
基体Al2O3粉末65％～79％，矿化剂MgO粉末2％～6％，成孔剂8％～12％，增塑剂10％～15％，碳纳米管1％～2％。
2.根据权利要求1所述的碳纳米管增强的多孔陶瓷型芯，其特征在于，所述成孔剂为淀粉。
3.根据权利要求1所述的碳纳米管增强的多孔陶瓷型芯，其特征在于，所述增塑剂为石蜡。
4.根据权利要求1所述的碳纳米管增强的多孔陶瓷型芯，其特征在于，所述Al2O3粉末粒度为180目的占60％-65％，粒度为280目的占35％-40％。
5.根据权利要求1所述的碳纳米管增强的多孔陶瓷型芯，其特征在于，所述MgO粉末的粒度为240目。
6.根据权利要求1所述的碳纳米管增强的多孔陶瓷型芯，其特征在于，所述碳纳米管属于直管型单壁碳纳米管，碳纳米管的长度直径比大于25:1。
7.一种权利要求1所述的碳纳米管增强的多孔陶瓷型芯的制备方法，其特征在于，具体按照以下步骤实施：
步骤1，各成分按照对应质量比称取，先将增塑剂石蜡加热到60℃～70℃，再按照上述比例加入Al2O3粉末、MgO粉末、淀粉和碳纳米管并不断搅拌，搅拌时间3h-4h，得到混合均匀的浆料；
步骤2，将混合均匀的浆料加入到热压注机，制备陶瓷型芯坯体；
步骤3，将制得的陶瓷型芯坯体冷冻干燥；
步骤4，将步骤3得到的陶瓷型芯坯体埋在氧化铝的刚玉匣钵中，进行烧结，得到目标碳纳米管增强的多孔陶瓷型芯。
8.根据权利要求7所述的碳纳米管增强的多孔陶瓷型芯的制备方法，其特征在于，在所述步骤2中，热压注机模具预热温度50℃～60℃，注射压力12Mpa～15Mpa，压注时间15s～17s。
9.根据权利要求7所述的碳纳米管增强的多孔陶瓷型芯的制备方法，其特征在于，在所述步骤3中，冷冻干燥的为温度-46～-50℃，时间为5h。
10.根据权利要求7所述的碳纳米管增强的多孔陶瓷型芯的制备方法，其特征在于，在所述步骤4中，烧结具体为：先室温升至420℃～450℃，升温速率4℃/min～5℃/min，保温时间2h；之后升温至900℃～920℃，升温速率8℃/min～10℃/min，保温时间1h；再升温至1770℃～1780℃，升温速率8℃/min～10℃/min，保温时间3h，然后断电，随炉冷却。
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