CN111087247A - 抑制陶瓷材料晶粒长大的方法及其应用 - Google Patents
抑制陶瓷材料晶粒长大的方法及其应用 Download PDFInfo
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Abstract
本发明提供了一种抑制陶瓷材料晶粒长大的方法及其应用。本发明提供的抑制陶瓷材料晶粒长大的方法包括将1)陶瓷材料的纳米粉体与微米粉体混合,得到混合粉体;2)将所述混合粉体制备成坯体;3)将所述坯体煅烧,得到所述陶瓷材料。采用本发明的方法制备的陶瓷材料有利于烧结致密化,抑制晶粒长大,同时提高材料的性能和强度。
Description
技术领域
本发明涉及一种抑制陶瓷材料晶粒长大的方法及其应用。
背景技术
能源和环境是全人类在21世纪中面临的重大课题。近年来,混合电导钙钛矿以及萤石矿陶瓷材料引起了化学、材料及物理等领域的科研工作者的广泛关注。其中混合电导钙钛矿陶瓷材料可以用作透氧膜材料和固体氧化物燃料电池的电极、连接体材料,萤石矿陶瓷材料可以应用于固体氧化物燃料电池的电解质材料,二者均具有很好的发展前景。
这两类材料应用时均需要在保证致密度基础上要有均匀的小晶粒。高温下,粉体的致密化与材料性能和工艺过程等因素有关,如粉体反应活性、纯度、形态、坯体密度、温度、时间、气氛等。但是如果采用纳米粉体则成本很高,不适宜工业化。如果采用固相合成方法制备的微米粉体再通过高能球磨,同样增加成本。直接采用微米粉体高温烧结后很难制备小晶粒的致密瓷体。已知的是有人采用加入助烧剂降低烧结温度,也有人加入其它种类的抑制剂抑制晶粒长大,但这两种方法都有可能由于其它种类粉体的加入影响性能。
发明内容
针对上述情况,本发明提出了一种制备微晶粒致密陶瓷材料的方法。这种方法可以通过采用加入少量同种纳米粉体材料抑制陶瓷晶粒长大,并保证材料的致密度。
在第一方面,本发明提供了一种抑制陶瓷材料晶粒长大的方法,其包括以下步骤:
1)将陶瓷材料的纳米粉体与微米粉体混合,得到混合粉体;
2)将所述混合粉体制备成坯体;
3)将所述坯体煅烧,得到所述陶瓷材料。
根据本发明的一些实施方式,所述纳米粉体与微米粉体来自于同种陶瓷材料。
根据本发明的一些实施方式,所述纳米粉体的粒径为1-100nm,例如5nm、15nm、25nm、35nm、45nm、55nm、65nm、75nm、85nm、95nm。
根据本发明的优选实施方式,所述纳米粉体的粒径为1-50nm。
根据本发明的优选实施方式,所述纳米粉体的粒径为2-20nm。
根据本发明的一些实施方式,所述微米粉体的粒径为0.1-100μm,例如1μm、5μm、15μm、25μm、35μm、45μm、55μm、65μm、75μm、85μm、95μm。
根据本发明的优选实施方式,所述微米粉体的粒径为0.1-50μm。
根据本发明的优选实施方式,所述微米粉体的粒径为1-20μm。
根据本发明的一些实施方式,所述纳米粉体占混合粉体总量的0.1wt%-99.9wt%,例如0.5wt%、1wt%、1.5wt%、2wt%、2.5wt%、3wt%、3.5wt%、4wt%、4.5wt%、10wt%、20wt%、30wt%、40wt%、50wt%、60wt%、70wt%、80wt%、90wt%。
根据本发明的优选实施方式,所述纳米粉体占混合粉体总量的0.1wt%-50wt%。
根据本发明的优选实施方式,所述纳米粉体占混合粉体总量的0.1wt%-5wt%。
根据本发明的一些实施方式,步骤1)中,通过球磨法将陶瓷材料的纳米粉体与微米粉体混合。
根据本发明的一些实施方式,步骤1)中,所述混合的时间为10-30h。
根据本发明的优选实施方式,步骤1)中,所述混合的时间为20-30h。
根据本发明的一些实施方式,步骤2)中,所述混合粉体通过选自压制、流延和挤出中的任意一种方式制备成坯体。
根据本发明的一些实施方式,所述煅烧的温度为500-1600℃。
根据本发明的优选实施方式,所述煅烧的温度为1000-1350℃。
根据本发明的一些实施方式,所述煅烧的时间为2-10h。
根据本发明的一些实施方式,所述陶瓷材料的化学组成为A′1-xA″xB′1-yB″yO3-δ,其中,A′和A″不同,各自独立地选自镧系元素,B′和B″不同,各自独立地选自第三周期、第四周期、第五周期元素,0≤x≤1,0≤y≤1。
根据本发明的优选实施方式,A′和A″不同,各自独立地选自La、Pr、Sr、Gd、Yb、Ce和Sm。
根据本发明的优选实施方式,B′和B″不同,各自独立地选自Y、Zr、Sc、Ga和Mg。
根据本发明的一些实施方式,所述陶瓷材料选自3-20mol%Y2O3稳定的ZrO2、3-20mol%Sc2O3稳定的ZrO2(SSZ)、GdxCe1-xO2-δ(GDC)、SmxCe1-xO2-δ(SDC)、YxCe1-xO2-δ(YDC)、LaxCe1-xO2-δ(LDC)、La1-xSrxGa1-yMgyO3-δ(LSGM)和Ba1-z(Ce0.7Zr0.1Y0.2-wYbw)O3-δ(BZCYYb)中的至少一种,其中0<x<1,0<y<1,0≤w≤0.2,0≤z≤0.2。
在第二方面,本发明提供了一种根据第一方面所述的方法得到的陶瓷材料。
根据本发明的一些实施方式,所述陶瓷材料的晶粒的粒径为0.1-10μm。
根据本发明的优选实施方式,所述陶瓷材料的晶粒的粒径为0.3-1μm。
在第三方面,本发明提供了一种根据第一方面所述的方法得到的陶瓷材料或根据第二方面所述的陶瓷材料在透氧膜材料或燃料电池中电解质和连接体材料中的应用。
根据本发明的一些实施方式,所述燃料电池为固体氧化物燃料电池。
本发明提供了一种通过采用加入少量同种纳米粉体材料抑制陶瓷晶粒长大的方法。根据本发明的一组实施例,对比了直接采用微米级粉体制备钙钛矿陶瓷材料与采用加入同种少量纳米级粉体在同样烧结制度下制备的钙钛矿陶瓷材料微观结构图。结果显示,其中加入同种少量纳米粉体烧结后,晶粒明显减小。采用此种方法制备的陶瓷材料有利于烧结致密化,抑制晶粒长大,同时提高材料的性能和强度。
附图说明
图1为根据实施例1制备的陶瓷材料的微观结构图。
图2为根据对比例1制备的陶瓷材料的微观结构图。
具体实施方式
下面结合实施例,进一步说明本发明。
实施例1
加入5wt%纳米La0.7Ca0.3Cr0.95Zn0.05O3-δ(LCCZ)粉体(粒径为2-20nm)与95wt%微米级LCCZ粉体(粒径为1-20μm)采用行星球磨机混合球磨24小时,取出烘干,然后采用压机在200MPa压力下干压后,在马弗炉中1300℃烧结5h,制备得到陶瓷材料。所得陶瓷材料的晶粒粒径平均为0.3-1μm,其微观结构图如图1所示。
对比例1
同样条件下,采用微米级La0.7Ca0.3Cr0.95Zn0.05O3-δ(LCCZ)粉体(粒径为1-20μm)干压后、1300℃烧结5h制备的陶瓷材料。所得陶瓷材料的晶粒粒径平均为0.5-10μm,其微观结构图如图2所示。
根据图1和图2所示,对比直接采用微米级粉体制备钙钛矿陶瓷材料与采用加入同种少量纳米级粉体在同样烧结制度下制备的钙钛矿陶瓷材料微观结构图,结果显示,在其中加入同种少量纳米粉体烧结后,晶粒明显减小。
应当注意的是,以上所述的实施例仅用于解释本发明,并不构成对本发明的任何限制。通过参照典型实施例对本发明进行了描述,但应当理解为其中所用的词语为描述性和解释性词汇,而不是限定性词汇。可以按规定在本发明权利要求的范围内对本发明作出修改,以及在不背离本发明的范围和精神内对本发明进行修订。尽管其中描述的本发明涉及特定的方法、材料和实施例,但是并不意味着本发明限于其中公开的特定例,相反,本发明可扩展至其他所有具有相同功能的方法和应用。
Claims (10)
1.一种抑制陶瓷材料晶粒长大的方法,其包括以下步骤:
1)将陶瓷材料的纳米粉体与微米粉体混合,得到混合粉体;
2)将所述混合粉体制备成坯体;
3)将所述坯体煅烧,得到所述陶瓷材料。
2.根据权利要求1所述的方法,其特征在于,所述纳米粉体与微米粉体来自于同种陶瓷材料。
3.根据权利要求1或2所述的方法,其特征在于,所述纳米粉体的粒径为1-100nm,优选为1-50nm,更优选为2-20nm;和/或所述微米粉体的粒径为0.1-100μm,优选为0.1-50μm,更优选为1-20μm。
4.根据权利要求1-3中任一项所述的方法,其特征在于,所述纳米粉体占混合粉体总量的0.1wt%-99.9wt%,优选为0.1-50wt%,更优选为0.1wt%-5wt%。
5.根据权利要求1-4中任一项所述的方法,其特征在于,步骤1)中,通过球磨法将陶瓷材料的纳米粉体与微米粉体混合,优选地,所述混合的时间为10-30h,更优选为20-30h;和/或
步骤2)中,通过选自压制、流延和挤出中的任意一种方式将所述混合粉体制备成坯体。
6.根据权利要求1-5中任一项所述的方法,其特征在于,所述煅烧的温度为500-1600℃,优选为1000-1350℃;时间为2-10小时。
7.根据权利要求1-6中任一项所述的方法,其特征在于,所述陶瓷材料的化学组成为A′1-xA″xB′1-yB″yO3-δ,其中,A′和A″不同,各自独立地选自镧系元素,优选选自La、Pr、Sr、Gd、Yb、Ce和Sm;B′和B″不同,各自独立地选自第三周期、第四周期、第五周期元素,优选选自Y、Zr、Sc、Ga和Mg;其中0≤x≤1,0≤y≤1。
8.根据权利要求1-7中任一项所述的方法,其特征在于,所述陶瓷材料选自3-20mol%Y2O3稳定的ZrO2、3-20mol%Sc2O3稳定的ZrO2、GdxCe1-xO2-δ、SmxCe1-xO2-δ、YxCe1-xO2-δ、LaxCe1- xO2-δ、La1-xSrxGa1-yMgyO3-δ和Ba1-z(Ce0.7Zr0.1Y0.2-wYbw)O3-δ中的至少一种,其中0<x<1,0<y<1,0≤w≤0.2,0≤z≤0.2。
9.一种根据权利要求1-8中任一项所述的方法得到的陶瓷材料,其特征在于,所述陶瓷材料的晶粒的粒径为0.1-10μm,优选为0.3-1μm。
10.一种根据权利要求1-8中任一项所述的方法得到的陶瓷材料或根据权利要求9所述的陶瓷材料在透氧膜材料或燃料电池中电解质和连接体材料中的应用。
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