CN108083779B - 一种稀土氧化铝陶瓷复合材料及其制备方法 - Google Patents
一种稀土氧化铝陶瓷复合材料及其制备方法 Download PDFInfo
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Abstract
本发明提出一种稀土氧化铝陶瓷复合材料及其制备方法,以氧化铝为基材,以氧化钇、二氧化钛为烧结助剂,以混合稀土氧化物对材料进行改性、增韧,来提高其力学性能,增强其韧性,提高抗折强度和材料硬度,形成先进的陶瓷基复合材料体系,并对其混合稀土助剂的组成,材料的成型方法,烧结方法,连接方法,粘结剂的使用做了***的研究。降低了材料的生产成本,并提高了复合材料的整体性能和可加工性,使其能方便的生产外形和尺寸复杂的陶瓷结构工件。
Description
技术领域
本发明属于先进陶瓷材料领域,涉及稀土氧化铝陶瓷复合材料的组分设计,制备方法及该材料达到的技术指标。
背景技术
氧化铝陶瓷材料具有高硬度、耐高温、高压,抗腐蚀,抗冲击,耐腐蚀、耐磨损等特点,已广泛应用于机械、也进、化工、医疗等各个领域。但因韧性、脆性、强度有待提高,而影响了它的使用寿命和更广泛的应用。
山东大学张希华等研究了92氧化铝中稀土改性增韧补强氧化铝基陶瓷复合材料的机理,认为加入稀土元素可以明显改善陶瓷材料的力学性能,有较好的增韧效果。汕头大学程西云等研究了稀土对陶瓷涂层的改性作用后认为,稀土元素可以提高陶瓷涂层的抗热震性,并可提高陶瓷涂层的硬度、抗高温性、耐蚀性和耐磨性,改善陶瓷涂层的断裂韧性。南京工业大学姚义俊等研究了稀土氧化物对氧化铝陶瓷性能的影响后认为,稀土氧化物的加入降低了95氧化铝瓷的烧结温度,抗弯强度和断裂韧性得到提高。佳木斯大学张敬强等研究了稀土氧化物对陶瓷纤维结构和力学性能影响后认为,稀土氧化物的加入对材料显微结构和力学性能有较大的影响,增韧机制主要是裂纹桥联、分叉、偏转以及裂纹尖端的桥联和断裂过程中的晶粒拔出机制带来的增韧效应,其断裂韧性得到很大的提高。
航空发动机点火***具有严苛的使用环境,而且零部件结构形状复杂,目前使用的95氧化铝陶瓷材料,采用Al-Si-Ca系组分,热压注成型技术,高温下烧结后形成多晶多相的致密陶瓷体,瓷体在点火***产品中装配,在航空发动机工作工况下表现出断裂韧性较低,显示脆性较大,限制了该氧化铝陶瓷材料的进一步应用。
发明内容
为解决现有技术存在的问题,本发明提出一种稀土氧化铝陶瓷复合材料及其制备方法,以氧化铝为基材,以氧化钇、二氧化钛为烧结助剂,以混合稀土氧化物对材料进行改性、增韧,来提高其力学性能,增强其韧性,提高抗折强度和材料硬度,形成先进的陶瓷基复合材料体系,并对其混合稀土助剂的组成,材料的成型方法,烧结方法,连接方法,粘结剂的使用做了***的研究。降低了材料的生产成本,并提高了复合材料的整体性能和可加工性,使其能方便的生产外形和尺寸复杂的陶瓷结构工件。
本发明的技术方案为:
所述一种稀土氧化铝陶瓷复合材料,其特征在于:由以下重量百分比的原料制成:90%-92%的稀土陶瓷粉料,6%-8%的混合粘结剂,1%-3%的水;
其中稀土陶瓷粉料由以下重量百分比的原材料制成:氧化铝94%-96%,二氧化钛0.3%-0.5%,氧化钇0.35%-0.5%,碳化硅纤维0.5%-1.5%,稀土混合助剂2.5%-3.5%;所述稀土混合助剂由氧化镧、氧化铈、氧化钕、氧化钐和氧化镨组成。
进一步的优选方案,所述一种稀土氧化铝陶瓷复合材料,其特征在于:所述混合粘结剂由PUA试剂中溶入石蜡和蜂蜡制备而成。
进一步的优选方案,所述一种稀土氧化铝陶瓷复合材料的制备方法,其特征在于:所述混合粘结剂由在质量浓度为50%的PUA试剂加入石蜡和蜂蜡制备而成,石蜡和蜂蜡的总质量占混合粘结剂总质量的8%。
所述一种稀土氧化铝陶瓷复合材料的制备方法,其特征在于:包括以下步骤:
步骤1:原材料预处理:
氧化铝预处理:对氧化铝粉体进行热处理,使其晶相由β-Al2O3转变成α-Al2O3,对热处理后的氧化铝粉体进行研磨,粒度小于1000目筛;
二氧化钛预处理:对二氧化钛进行热处理,使锐钛型二氧化钛转化成金红型二氧化钛,对热处理后的二氧化钛进行研磨,粒度小于500目筛;
氧化钇预处理:对氧化钇进行研磨,粒度小于400目筛;
稀土混合助剂处理:对稀土混合助剂进行研磨,粒度小于600目筛;
步骤2:按照氧化铝94%-96%,二氧化钛0.3%-0.5%,氧化钇0.35%-0.5%,碳化硅纤维0.5%-1.5%,稀土混合助剂2.5%-3.5%的配比,将步骤1处理后的氧化铝、二氧化钛、氧化钇、稀土混合助剂以及碳化硅纤维滚磨混合,过100目筛得到稀土陶瓷粉料;
步骤3:按照90%-92%的稀土陶瓷粉料,6%-8%的混合粘结剂,1%-3%的水的配比,在稀土陶瓷粉料中加入混合粘结剂和水,形成预制料,预制料搅拌均匀后,干燥,破碎,得到粒度为0.08mm-0.3mm的造粒粉;
步骤4:将造粒粉装入模具中,等静压成型得到毛坯;将毛坯烧结成瓷或对毛坯进行进一步车削加工后再烧结成瓷。
进一步的优选方案,所述一种稀土氧化铝陶瓷复合材料的制备方法,其特征在于:二氧化钛预处理过程中,对二氧化钛进行热处理的过程为:
首先以200℃/h的升温速率从室温升至600℃,再以150℃/h的升温速率从600℃升至800℃,再以80℃/h的升温速率从800℃升至950℃,在950±10℃下保温2h。
进一步的优选方案,所述一种稀土氧化铝陶瓷复合材料的制备方法,其特征在于:步骤4中在1640℃-1660℃下烧结成瓷。
进一步的优选方案,所述一种稀土氧化铝陶瓷复合材料的制备方法,其特征在于:氧化铝预处理过程中,采用浓度50%的三乙醇胺作为研磨剂,研磨剂质量占氧化铝质量的3%-5%.
进一步的优选方案,所述一种稀土氧化铝陶瓷复合材料的制备方法,其特征在于:步骤4中造粒粉装入模具后,在150MPa压力下等静压成型得到毛坯。
有益效果
本发明提供了一种混合稀土助剂增韧补强氧化铝陶瓷复合材料及其制备方法。本发明提高了95氧化铝陶瓷材料的力学性能,断裂韧性和硬度;本发明提供的复合材料显微结构得到明显改善,其抗热震性也有提高。其特性对比见表1。
本发明的复合材料,其抗折强度比目前使用的95氧化铝陶瓷提高2.5倍以上,断裂韧性提高4倍以上,其力学性能明显提高,硬度得到提高,抗热震性得到提高,显微结构得到改善,材料整体性能得到提升,提高了材料的使用可靠性、耐久性和安全性。本发明的制备方法采用冷等静压成型,毛坯车削,无压烧结技术,具有工艺简单,生产周期更短,成本低,便于制造构建,便于大规模生产的特点。
本发明所涉及的稀土混合助剂明显改善复合材料的力学性能和显微结构,降低复合材料的烧结温度;所涉及的混合粘结剂不仅有利于成型,而且利于车削,在车削时毛坯不断裂,不掉块,不崩角;所涉及的碳化硅纤维改善了复合材料的显微结构,增强了韧性,使抗热震性提高;所涉及的氧化钇明显降低了复合材料的烧结温度。
本发明提供的制备方法,降低了复合材料的生产成本,并提高了复合材料的整体性能和可加工性,使其能方便的生产外形和尺寸不限的陶瓷结构工件。
表1稀土氧化铝陶瓷复合材料与95氧化铝陶瓷材料特性对比表
本发明的附加方面和优点将在下面的描述中部分给出,部分将从下面的描述中变得明显,或通过本发明的实践了解到。
具体实施方式
下面详细描述本发明的实施例,所述实施例是示例性的,旨在用于解释本发明,而不能理解为对本发明的限制。
本发明旨在通过加入稀土混合助剂,明显改善材料的力学性能和显微结构,加入氧化钛和氧化钇改善其烧结热力学性能,研制出一种适合发动机工作环境的先进陶瓷基复合材料。
其中稀土氧化铝陶瓷复合材料成型用的造粒粉由以下重量百分比的原料制成:90%-92%的稀土陶瓷粉料,6%-8%的混合粘结剂,1%-3%的水。造粒粉经等静压成型后,在车床上车削成所需构建外形,常压下烧结成瓷。
其中稀土陶瓷粉料由以下重量百分比的原材料制成:氧化铝94%-96%,二氧化钛0.3%-0.5%,氧化钇0.35%-0.5%,碳化硅纤维0.5%-1.5%,稀土混合助剂2.5%-3.5%;所述稀土混合助剂由氧化镧、氧化铈、氧化钕、氧化钐和氧化镨组成。
具体的复合材料的制备技术流程如下:
步骤1:原材料预处理:
氧化铝预处理:将氧化铝粉体在1450℃进行热处理,使其晶相由β-Al2O3全部转变成α-Al2O3,对热处理后的氧化铝粉体在行星式球磨机上球磨不小于25h,使其粒度小于1000目筛;其中采用浓度50%的三乙醇胺作为研磨剂,研磨剂质量占氧化铝质量的3%-5%。
二氧化钛预处理:将二氧化钛在刚玉坩埚中进行热处理,使锐钛型二氧化钛全部转化成稳定的金红型二氧化钛,对热处理后的金红型二氧化钛在行星式球磨机上球磨不小于5h,使其粒度小于500目筛。对二氧化钛进行热处理的过程为:
首先以200℃/h的升温速率从室温升至600℃,再以150℃/h的升温速率从600℃升至800℃,再以80℃/h的升温速率从800℃升至950℃,在950±10℃下保温2h。
氧化钇预处理:将氧化钇在行星式球磨机上球磨不小于5h,使其粒度小于400目筛。氧化钇Y2O3能够促进烧结,存在于氧化铝的晶界上,降低晶界迁移速率,抑制晶粒长大,使晶粒大小均匀形成致密纤维结构。
稀土混合助剂处理:采用行星式球磨机对稀土混合助剂进行研磨,粒度小于600目筛。
混合稀土离子助剂有助于改善氧化铝陶瓷的显微结构,提高瓷体的抗折强度和韧性,适当的粒度分布有助于烧结的进行。
La2O3提高材料的致密度,显著提高材料断裂韧性;Sm2O3催进材料烧结,显著缩短保温时间,利于材料致密化;CeO2提高材料体积电阻率,陶瓷断裂路径曲折,裂纹出现架桥、分叉现象,使断裂能提高,从而提高材料的力学性能;Pr2O3、La2O3、Sm2O3和Nd2O3可大大改善材料的介电性和压电性;La2O3、Nd2O3和CeO2可有效移动居里点。通过五种稀土离子混合得到的混合稀土离子助剂能够有效提高氧化铝陶瓷基复合材料性能。
制备混合粘结剂:在质量浓度为50%的PUA试剂(聚酯聚氨酯丙烯酸)中溶入石蜡和蜂蜡制备成混合粘结剂,密封储存备用。石蜡和蜂蜡的总质量占混合粘结剂总质量的8%。
步骤2:按照氧化铝94%-96%,二氧化钛0.3%-0.5%,氧化钇0.35%-0.5%,碳化硅纤维0.5%-1.5%,稀土混合助剂2.5%-3.5%的配比,将步骤1处理后的氧化铝、二氧化钛、氧化钇、稀土混合助剂以及碳化硅纤维混合后在球磨滚筒中滚磨混合不小于0.5h,过100目筛得到稀土陶瓷粉料。
步骤3:按照90%-92%的稀土陶瓷粉料,6%-8%的混合粘结剂,1%-3%的水的配比,在稀土陶瓷粉料中加入混合粘结剂和水,形成预制料,预制料搅拌均匀后,干燥,破碎,得到粒度为0.08mm-0.3mm的造粒粉;造粒粉是假性颗粒,利于装料和压制毛坯。
步骤4:将造粒粉装入模具中,在150MPa压力下等静压成型,形成所需要的形状和结构的毛坯;等静压成型压力均匀而且赋予粉料一定的毛坯形状和强度,便于后续加工。在数控车床上控制转速和车削量,将毛坯车削加工成所需要的构件尺寸,加工的目的是赋予毛坯一定的形状和尺寸精度;再在硅钼棒电炉中,常压下在1640℃-1660℃下烧结成瓷,得到稀土陶瓷复合材料零件。烧结的目的是赋予材料特有的显微结构,赋予工件特定的强度和特征功能。
最后按照GB5593检测材料的抗折强度,硬度,韧性,抗热震性,体积密度,抗电强度等。结果如表1所示,表明其抗折强度比目前使用的95氧化铝陶瓷提高2.5倍以上,断裂韧性提高4倍以上,其力学性能明显提高,硬度得到提高,抗热震性得到提高,显微结构得到改善,材料整体性能得到提升,提高了材料的使用可靠性、耐久性和安全性。本发明的制备方法采用冷等静压成型,毛坯车削,无压烧结技术,具有工艺简单,生产周期更短,成本低,便于制造构建,便于大规模生产的特点。
尽管上面已经示出和描述了本发明的实施例,可以理解的是,上述实施例是示例性的,不能理解为对本发明的限制,本领域的普通技术人员在不脱离本发明的原理和宗旨的情况下在本发明的范围内可以对上述实施例进行变化、修改、替换和变型。
Claims (8)
1.一种稀土氧化铝陶瓷复合材料,其特征在于:由以下重量百分比的原料制成:
90%-92%的稀土陶瓷粉料,6%-8%的混合粘结剂,1%-3%的水;
其中稀土陶瓷粉料由以下重量百分比的原材料制成:氧化铝94%-96%,二氧化钛0.3%-0.5%,氧化钇0.35%-0.5%,碳化硅纤维0.5%-1.5%,稀土混合助剂2.5%-3.5%;所述稀土混合助剂由氧化镧、氧化铈、氧化钕、氧化钐和氧化镨组成。
2.根据权利要求1所述一种稀土氧化铝陶瓷复合材料,其特征在于:所述混合粘结剂由PUA试剂中溶入石蜡和蜂蜡制备而成。
3.根据权利要求2所述一种稀土氧化铝陶瓷复合材料的制备方法,其特征在于:所述混合粘结剂由在质量浓度为50%的PUA试剂加入石蜡和蜂蜡制备而成,石蜡和蜂蜡的总质量占混合粘结剂总质量的8%。
4.一种稀土氧化铝陶瓷复合材料的制备方法,其特征在于:包括以下步骤:
步骤1:原材料预处理:
氧化铝预处理:对氧化铝粉体进行热处理,使其晶相由β-Al2O3转变成α-Al2O3,对热处理后的氧化铝粉体进行研磨,粒度小于1000目筛;
二氧化钛预处理:对二氧化钛进行热处理,使锐钛型二氧化钛转化成金红型二氧化钛,对热处理后的二氧化钛进行研磨,粒度小于500目筛;
氧化钇预处理:对氧化钇进行研磨,粒度小于400目筛;
稀土混合助剂处理:对稀土混合助剂进行研磨,粒度小于600目筛;
步骤2:按照氧化铝94%-96%,二氧化钛0.3%-0.5%,氧化钇0.35%-0.5%,碳化硅纤维0.5%-1.5%,稀土混合助剂2.5%-3.5%的配比,将步骤1处理后的氧化铝、二氧化钛、氧化钇、稀土混合助剂以及碳化硅纤维滚磨混合,过100目筛得到稀土陶瓷粉料;
步骤3:按照90%-92%的稀土陶瓷粉料,6%-8%的混合粘结剂,1%-3%的水的配比,在稀土陶瓷粉料中加入混合粘结剂和水,形成预制料,预制料搅拌均匀后,干燥,破碎,得到粒度为0.08mm-0.3mm的造粒粉;
步骤4:将造粒粉装入模具中,等静压成型得到毛坯;将毛坯烧结成瓷或对毛坯进行进一步车削加工后再烧结成瓷。
5.根据权利要求4所述一种稀土氧化铝陶瓷复合材料的制备方法,其特征在于:二氧化钛预处理过程中,对二氧化钛进行热处理的过程为:
首先以200℃/h的升温速率从室温升至600℃,再以150℃/h的升温速率从600℃升至800℃,再以80℃/h的升温速率从800℃升至950℃,在950±10℃下保温2h。
6.根据权利要求4所述一种稀土氧化铝陶瓷复合材料的制备方法,其特征在于:步骤4中在1640℃-1660℃下烧结成瓷。
7.根据权利要求4所述一种稀土氧化铝陶瓷复合材料的制备方法,其特征在于:氧化铝预处理过程中,采用浓度50%的三乙醇胺作为研磨剂,研磨剂质量占氧化铝质量的3%-5%。
8.根据权利要求4所述一种稀土氧化铝陶瓷复合材料的制备方法,其特征在于:步骤4中造粒粉装入模具后,在150MPa压力下等静压成型得到毛坯。
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