CN112062547A - 氮化铝/氧化铝复合陶瓷型芯及其制备方法 - Google Patents
氮化铝/氧化铝复合陶瓷型芯及其制备方法 Download PDFInfo
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Abstract
一种定向凝固用氮化铝/氧化铝复合陶瓷型芯的制备方法,将作为陶瓷型芯原料的电熔刚玉粉、球形氮化铝粉、高岭土、木质素纤维混合后加入增塑剂制成浆料,经压制和两阶段烧结后,再经硅酸乙酯水解液强化得到氮化铝/氧化铝复合陶瓷型芯;本发明得到的复合陶瓷型芯具有优良的抗热震性能以及较好的碱液溶解性能,能够承受1550℃‑1700℃的高温而变形量很小,在高温度梯度下不开裂,用于满足航空发动机和燃气轮机涡轮空心叶片定向凝固成形需求。
Description
技术领域
本发明涉及的是一种熔模铸造领域的技术,具体是一种氮化铝/氧化铝复合陶瓷型芯及其制备方法。
背景技术
陶瓷型芯用于在叶片的定向凝固成形过程中形成空心叶片的内腔,并与熔模及型壳共同保证空心叶片壁厚的尺寸精度,叶片成型后,再将型芯通过机械或化学方法去除,即可得到叶片的空心结构。由于陶瓷型芯在使用过程中,长时间浸泡在高温金属液中,除承受金属液的静压力外,还需要承受大的温度梯度所产生的应力,这对陶瓷型芯的抗高温蠕变性能、抗热震性能都提出了很高的要求。
现有技术有采用石英玻璃和氧化铝为主的硅基陶瓷型芯,其中氧化铝陶瓷型芯高温性能较好,但是其抗热冲击性能较差,且化学惰性强,采用碱液溶解速度远低于二氧化硅,且烧结温度仅为1250℃,很难保证氧化铝陶瓷型芯的烧结质量。
现有技术也提出了一些加速型芯脱除的工艺和设备方案,但是如果不能解决氧化铝陶瓷型芯本身的材质问题,也很难实现加速型芯脱除的目标。另一方面,由于氧化铝陶瓷型芯导热性能较差,抗热震性能不佳,因此在成形大尺寸空心叶片时,高的温度区间和高的温度梯度更容易造成氧化铝陶瓷型芯因应力-应变而断裂。上述问题的存在,大大限制了氧化铝陶瓷型芯的应用。
发明内容
本发明针对现有技术存在的上述不足,提出一种氮化铝/氧化铝复合陶瓷型芯及其制备方法,得到的复合陶瓷型芯具有优良的抗热震性能以及较好的碱液溶解性能,能够承受1550℃-1700℃的高温而变形量很小,在高温度梯度下不开裂,用于满足航空发动机和燃气轮机涡轮空心叶片定向凝固成形需求。
本发明是通过以下技术方案实现的:
本发明涉及一种氮化铝/氧化铝复合陶瓷型芯的制备方法,将作为陶瓷型芯原料的电熔刚玉粉、球形氮化铝粉、高岭土、木质素纤维混合后加入增塑剂制成浆料,经压制和两阶段烧结后,再经硅酸乙酯水解液强化得到氮化铝/氧化铝复合陶瓷型芯。
所述的陶瓷型芯原料中的组分及重量百分比具体为:70-80wt.%电熔刚玉粉、15-25wt.%的球形氮化铝粉、1-4wt.%高岭土、1-4wt.%木质素纤维。
所述的混合,优选采用V型混料机强制搅拌干混2-5h。
所述的增塑剂占芯料15-30wt.%,优选为熔融状态下与陶瓷型芯原料搅拌混合制成浆料。
所述的电熔刚玉粉,粒度分布为1-60μm,α-Al2O3含量不低于99wt.%,其中Na2O含量不高于0.10wt.%。
所述的球形氮化铝粉,粒度分布为3-30μm,AlN的含量不低于99wt.%,其中Al4C3、Al2O3、C等杂质的总含量不高于1wt.%。
所述的高岭土,粒度分布为1-38μm,是经1450℃煅烧下于大气中煅烧过的高岭土,最高温度下煅烧时间不低于2h。
所述的木质素纤维,直径为1-10μm,长度为50-500μm,是经偶联剂进行表面处理的木质素纤维,其处理方法是:将木质素纤维浸泡在偶联剂中,保持1h,之后将木质素纤维在120℃下烘干24h,即得到表面改性的木质素纤维。
所述的增塑剂,包含半精炼石蜡、蜂蜡、聚乙烯和油酸,其重量百分比配方优选为:80wt.%的石蜡、15wt.%的蜂蜡、3wt.%的聚乙烯和2wt.%的油酸。
所述的硅酸乙酯水解液,包括:硅酸乙酯、无水乙醇、异丙醇、丙二醇甲醚、酸性硅溶胶以及盐酸,其重量百分比优选为:硅酸乙酯31.3wt.%、无水乙醇25wt.%、异丙醇1.5wt.%、丙二醇甲醚13wt.%、酸性硅溶胶25.8wt.%、以及浓度为20wt.%的盐酸溶液0.4wt.%。
所述的压制是指:将浆料在压芯机上进行压制,压制温度为120-130℃,压力为2-4MPa,保压时间为20-30s。
所述的两阶段烧结是指:将压制好的型芯素坯置于陶瓷匣钵的轻质氧化镁粉中,在气氛保护烧结炉中分段烧结,具体为:第一阶段在空气中从室温焙烧至120℃,保温1h,升温速度为30℃/h;从120℃焙烧至300℃,保温2h,升温速度为30℃/h;从300℃焙烧至600℃,保温4h,升温速度为30℃/h;第二阶段在氮气中进行焙烧,从600℃焙烧至1450℃,保温6h,升温速度为60℃/h;最后随炉冷却至室温,得到型芯烧结体。
所述的型芯烧结体,优选在两阶段烧结后进行表面吹粉清理后,用型芯量具进行检测后修型。
所述的强化是指:将型芯烧结体浸泡于硅酸乙酯水解液中并烘干,优选置于装有硅酸乙酯水解液的容器中并置于负压环境中,使硅酸乙酯水解液能够渗透到型芯的孔隙当中,浸泡时间保持2h,然后摆放在架子上自然晾干24h,再在150℃下于大气中热处理2h,自然冷却至室温,即得到最终的型芯产品。
本发明涉及上述方法制备得到的氮化铝/氧化铝复合陶瓷型芯,其最主要的性能指标为:室温抗弯强度为38.39-45.23MPa,1550℃下的抗弯强度为31.12-36.45MPa,1550℃下的挠度为0.32-0.41mm,孔隙率为26.9-36.8%,脱芯率达到100%,氮气保护下的1000℃至室温(空气中冷却)的热震次数为8-12次。
技术效果
氮化铝的密度为3.23g/cm3,导热系数约为200W/(m·K),氧化铝的密度为3.9g/cm3,导热系数仅为35W/(m·K),可见氮化铝的导热性能远高于氧化铝,这一特性赋予了氮化铝/氧化铝复合陶瓷型芯具有比传统的氧化铝陶瓷型芯更好的抗热震性能。
本发明整体解决了现有陶瓷型芯的抗热震性能和脱芯性能较低的问题。
与现有技术相比,采用本发明的技术制备的叶片空心部位质量好,尺寸精度高,型芯易于脱除,因此在新一代航空发动机涡轮叶片制备方面具有广阔的应用前景,同时也可以应用于高性能燃气轮机的空心涡轮叶片定向凝固精密铸造中。
本发明通过在型芯中添加具有良好柔韧性烧失性能的木质素纤维,可以显著降低大尺寸型芯素坯冷却时的体积收缩,大幅度提高陶瓷型芯素坯的尺寸精度;同时在型芯烧结过程中,木质素纤维完全烧掉,使型芯中残留大量的开孔孔隙,有利于后续型芯的顺利碱液脱除。同时,氮化铝与氧化铝相比,易被高温的氢氧化钾/氢氧化钠水溶液所溶解。因此,综合来看,氮化铝/氧化铝复合陶瓷型芯比传统的氧化铝陶瓷型芯表现出更好的溶解脱芯性能。
具体实施方式
实施例1
本实施例包括以下步骤:
步骤1)型芯浆料制备:按照重量百分比将70wt.%电熔刚玉粉、25wt.%的球形氮化铝粉、1wt.%高岭土、4wt.%木质素纤维加入到V型混料机中,强制搅拌干混5h,得到陶瓷芯料;将占芯料30wt.%的增塑剂加入到真空搅拌釜中,加热到120℃,增塑剂熔融后,再将陶瓷芯料在搅拌的条件下加入到熔融的增塑剂中,待所有的陶瓷芯料加入完毕后,再在真空下搅拌混合12h,得到型芯浆料。
步骤2)型芯压制:将型芯浆料在压芯机上进行压制,压制温度为120℃,压力为4MPa,保压时间为20s。
步骤3)型芯烧结:将压制好的型芯素坯置于陶瓷匣钵的轻质氧化镁粉中,在气氛保护烧结炉中分段烧结。第一段在空气中进行焙烧,优化的过程是:从室温升到120℃,保温1h,升温速度为30℃/h;从120℃升到300℃,保温2h,升温速度为30℃/h;从300℃升到600℃,保温4h,升温速度为30℃/h。第二段是在氮气中进行焙烧,优化的过程是:将烧结炉进行抽真空,之后冲入氮气,然后从600℃升到1450℃,保温6h,升温速度为60℃/h;随炉冷却至室温,得到型芯烧结体。
步骤4)型芯修型:将烧结好的型芯进行表面吹粉清理后,用型芯量具进行检测后修型。
步骤5)型芯强化:将型芯放入装有硅酸乙酯水解液的容器中,然后将容器置于负压环境中,使硅酸乙酯水解液能够渗透到型芯的孔隙当中,浸泡时间保持2h,然后摆放在架子上自然晾干24h,再在150℃下于大气中热处理2h,自然冷却至室温,即得到最终的型芯产品。
经检测,本实施例制备得到的氮化铝/氧化铝复合陶瓷型芯的室温抗弯强度为38.39MPa,1550℃下的抗弯强度为31.12MPa,1550℃下的挠度为0.41mm,孔隙率为36.8%;经在脱芯液(NaOH水溶液)浓度50wt.%、压力2.8MPa、温度360℃的脱芯釜中进行8h的脱芯试验,脱芯率达到100%;氮气保护下的1000℃至室温(空气中冷却)的热震次数为12次。而以电熔刚玉粉制备的陶瓷型芯在室温抗弯强度为24.42MPa,1550℃的抗弯强度为18.98Mpa,1550℃的挠度为1.02mm,孔隙率18.48%;经在脱芯液(NaOH水溶液)浓度50wt.%、压力2.8MPa、温度360℃的脱芯釜中进行8h的脱芯试验,脱芯率仅为12.1wt.%;氮气保护下的1000℃至室温(空气中冷却)的热震次数为3次。
实施例2
本实施例包括以下步骤:
步骤1)型芯浆料制备:按照重量百分比将75wt.%电熔刚玉粉、19wt.%的球形氮化铝粉、3wt.%高岭土、3wt.%木质素纤维加入到V型混料机中,强制搅拌干混3.5h,得到陶瓷芯料;将占芯料25wt.%的增塑剂加入到真空搅拌釜中,加热到120℃,增塑剂熔融后,再将陶瓷芯料在搅拌的条件下加入到熔融的增塑剂中,待所有的陶瓷芯料加入完毕后,再在真空下搅拌混合12h,得到型芯浆料。
步骤2)型芯压制:将型芯浆料在压芯机上进行压制,压制温度为125℃,压力为3MPa,保压时间为25s。
步骤3)型芯烧结:将压制好的型芯素坯置于陶瓷匣钵的轻质氧化镁粉中,在气氛保护烧结炉中分段烧结。第一段在空气中进行焙烧,优化的过程是:从室温升到120℃,保温1h,升温速度为30℃/h;从120℃升到300℃,保温2h,升温速度为30℃/h;从300℃升到600℃,保温4h,升温速度为30℃/h。第二段是在氮气中进行焙烧,优化的过程是:将烧结炉进行抽真空,之后冲入氮气,然后从600℃升到1450℃,保温6h,升温速度为60℃/h;随炉冷却至室温,得到型芯烧结体。
步骤4)型芯修型:将烧结好的型芯进行表面吹粉清理后,用型芯量具进行检测后修型。
步骤5)型芯强化:将型芯放入装有硅酸乙酯水解液的容器中,然后将容器置于负压环境中,使硅酸乙酯水解液能够渗透到型芯的孔隙当中,浸泡时间保持2h,然后摆放在架子上自然晾干24h,再在150℃下于大气中热处理2h,自然冷却至室温,即得到最终的型芯产品。
经检测,本实施例制备得到的氮化铝/氧化铝复合陶瓷型芯的室温抗弯强度为41.22MPa,1550℃下的抗弯强度为34.21MPa,1550℃下的挠度为0.38mm,孔隙率为31.4%;经在脱芯液(NaOH水溶液)浓度50wt.%、压力2.8MPa、温度360℃的脱芯釜中进行8h的脱芯试验,脱芯率达到100%;氮气保护下的1000℃至室温(空气中冷却)的热震次数为11次。而以电熔刚玉粉制备的陶瓷型芯在室温抗弯强度为24.42MPa,1550℃的抗弯强度为18.98Mpa,1550℃的挠度为1.02mm,孔隙率18.48%;经在脱芯液(NaOH水溶液)浓度50wt.%、压力2.8MPa、温度360℃的脱芯釜中进行8h的脱芯试验,脱芯率仅为12.1wt.%;氮气保护下的1000℃至室温(空气中冷却)的热震次数为3次。
实施例3
本实施例包括以下步骤:
步骤1)型芯浆料制备:按照重量百分比将80wt.%电熔刚玉粉、15wt.%的球形氮化铝粉、4wt.%高岭土、1wt.%木质素纤维加入到V型混料机中,强制搅拌干混3h,得到陶瓷芯料;将占芯料20wt.%的增塑剂加入到真空搅拌釜中,加热到120℃,增塑剂熔融后,再将陶瓷芯料在搅拌的条件下加入到熔融的增塑剂中,待所有的陶瓷芯料加入完毕后,再在真空下搅拌混合12h,得到型芯浆料。
步骤2)型芯压制:将型芯浆料在压芯机上进行压制,压制温度为130℃,压力为2MPa,保压时间为20s。
步骤3)型芯烧结:将压制好的型芯素坯置于陶瓷匣钵的轻质氧化镁粉中,在气氛保护烧结炉中分段烧结。第一段在空气中进行焙烧,优化的过程是:从室温升到120℃,保温1h,升温速度为30℃/h;从120℃升到300℃,保温2h,升温速度为30℃/h;从300℃升到600℃,保温4h,升温速度为30℃/h。第二段是在氮气中进行焙烧,优化的过程是:将烧结炉进行抽真空,之后冲入氮气,然后从600℃升到1450℃,保温6h,升温速度为60℃/h;随炉冷却至室温,得到型芯烧结体。
步骤4)型芯修型:将烧结好的型芯进行表面吹粉清理后,用型芯量具进行检测后修型。
步骤5)型芯强化:将型芯放入装有硅酸乙酯水解液的容器中,然后将容器置于负压环境中,使硅酸乙酯水解液能够渗透到型芯的孔隙当中,浸泡时间保持2h,然后摆放在架子上自然晾干24h,再在150℃下于大气中热处理2h,自然冷却至室温,即得到最终的型芯产品。
经检测,本实施例制备得到的氮化铝/氧化铝复合陶瓷型芯的室温抗弯强度为45.23MPa,1550℃下的抗弯强度为36.45MPa,1550℃下的挠度为0.32mm,孔隙率为26.9%;经在脱芯液(NaOH水溶液)浓度50wt.%、压力2.8MPa、温度360℃的脱芯釜中进行8h的脱芯试验,脱芯率达到100%;氮气保护下的1000℃至室温(空气中冷却)的热震次数为8次。而以电熔刚玉粉制备的陶瓷型芯在室温抗弯强度为24.42MPa,1550℃的抗弯强度为18.98Mpa,1550℃的挠度为1.02mm,孔隙率18.48%;经在脱芯液(KOH水溶液)浓度50wt.%、压力2.8MPa、温度360℃的脱芯釜中进行8h的脱芯试验,脱芯率仅为12.1wt.%;氮气保护下的1000℃至室温(空气中冷却)的热震次数为3次。
综上,本发明通过添加氮化铝和木质素纤维,使氮化铝/氧化铝复合陶瓷型芯获得了优良的抗热震性能,且显著提高了型芯的脱除性能。
与现有技术相比,本发明的氮化铝/氧化铝复合陶瓷型芯室温抗弯强度为38.39-45.23MPa,1550℃下的抗弯强度为31.12-36.45MPa,1550℃下的挠度为0.32-0.41mm,孔隙率为26.9-36.8%,脱芯率达到100%,氮气保护下的1000℃至室温(空气中冷却)的热震次数为8-12次。而以电熔刚玉粉制备的陶瓷型芯在室温抗弯强度为24.42MPa,1550℃的抗弯强度为18.98Mpa,1550℃的挠度为1.02mm,孔隙率18.48%,脱芯率仅为12.1wt.%;氮气保护下的1000℃至室温(空气中冷却)的热震次数为3次。本发明的氮化铝/氧化铝复合陶瓷型芯具备更优良的性能指标。
上述具体实施可由本领域技术人员在不背离本发明原理和宗旨的前提下以不同的方式对其进行局部调整,本发明的保护范围以权利要求书为准且不由上述具体实施所限,在其范围内的各个实现方案均受本发明之约束。
Claims (10)
1.一种定向凝固用氮化铝/氧化铝复合陶瓷型芯的制备方法,其特征在于,将作为陶瓷型芯原料的电熔刚玉粉、球形氮化铝粉、高岭土、木质素纤维混合后加入增塑剂制成浆料,经压制和两阶段烧结后,再经硅酸乙酯水解液强化得到氮化铝/氧化铝复合陶瓷型芯;
所述的强化是指:将型芯烧结体浸泡于硅酸乙酯水解液中并烘干。
2.根据权利要求1所述的氮化铝/氧化铝复合陶瓷型芯的制备方法,其特征是,所述的陶瓷型芯原料中的组分及重量百分比具体为:70-80wt.%电熔刚玉粉、15-25wt.%的球形氮化铝粉、1-4wt.%高岭土、1-4wt.%木质素纤维。
3.根据权利要求1所述的氮化铝/氧化铝复合陶瓷型芯的制备方法,其特征是,所述的增塑剂占芯料15-30wt.%,该增塑剂为熔融状态下与陶瓷型芯原料搅拌混合制成浆料。
4.根据权利要求1或2所述的氮化铝/氧化铝复合陶瓷型芯的制备方法,其特征是,所述的电熔刚玉粉,粒度分布为1-60μm,α-Al2O3含量不低于99wt.%,其中Na2O含量不高于0.10wt.%;
所述的球形氮化铝粉,粒度分布为3-30μm,AlN的含量不低于99wt.%,其中Al4C3、Al2O3、C等杂质的总含量不高于1wt.%;
所述的高岭土,粒度分布为1-38μm,是经1450℃煅烧下于大气中煅烧过的高岭土,最高温度下煅烧时间不低于2h;
所述的木质素纤维,直径为1-10μm,长度为50-500μm,是经偶联剂进行表面处理的木质素纤维,其处理方法是:将木质素纤维浸泡在偶联剂中,保持1h,之后将木质素纤维在120℃下烘干24h,即得到表面改性的木质素纤维。
5.根据权利要求3所述的氮化铝/氧化铝复合陶瓷型芯的制备方法,其特征是,所述的增塑剂,包含半精炼石蜡、蜂蜡、聚乙烯和油酸,其重量百分比配方为:80wt.%的石蜡、15wt.%的蜂蜡、3wt.%的聚乙烯和2wt.%的油酸。
6.根据权利要求1所述的氮化铝/氧化铝复合陶瓷型芯的制备方法,其特征是,所述的硅酸乙酯水解液,包括:硅酸乙酯、无水乙醇、异丙醇、丙二醇甲醚、酸性硅溶胶以及盐酸。
7.根据权利要求1或6所述的氮化铝/氧化铝复合陶瓷型芯的制备方法,其特征是,所述的硅酸乙酯水解液的重量百分比为:硅酸乙酯31.3wt.%、无水乙醇25wt.%、异丙醇1.5wt.%、丙二醇甲醚13wt.%、酸性硅溶胶25.8wt.%、以及浓度为20wt.%的盐酸溶液0.4wt.%。
8.根据权利要求1所述的氮化铝/氧化铝复合陶瓷型芯的制备方法,其特征是,所述的两阶段烧结是指:将压制好的型芯素坯置于陶瓷匣钵的轻质氧化镁粉中,在气氛保护烧结炉中分段烧结,具体为:第一阶段在空气中从室温焙烧至120℃,保温1h,升温速度为30℃/h;从120℃焙烧至300℃,保温2h,升温速度为30℃/h;从300℃焙烧至600℃,保温4h,升温速度为30℃/h;第二阶段在氮气中进行焙烧,从600℃焙烧至1450℃,保温6h,升温速度为60℃/h;最后随炉冷却至室温,得到型芯烧结体。
9.根据权利要求1所述的氮化铝/氧化铝复合陶瓷型芯的制备方法,其特征是,所述的强化是指:将型芯烧结体置于装有硅酸乙酯水解液的容器中并置于负压环境中,使硅酸乙酯水解液能够渗透到型芯的孔隙当中,浸泡时间保持2h,然后摆放在架子上自然晾干24h,再在150℃下于大气中热处理2h,自然冷却至室温,即得到最终的型芯产品。
10.一种基于上述任一权利要求所述方法制备得到的氮化铝/氧化铝复合陶瓷型芯,其特征在于,其室温抗弯强度为38.39-45.23MPa,1550℃下的抗弯强度为31.12-36.45MPa,1550℃下的挠度为0.32-0.41mm,孔隙率为26.9-36.8%,脱芯率达到100%,氮气保护下的1000℃至室温的热震次数为8-12次。
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