CN113185305B - 一种高温隔热高熵氧化物及其制备方法 - Google Patents
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Abstract
本发明公开了一种高温隔热高熵氧化物及其制备方法,该高温隔热高熵氧化物结构为立方萤石相,化学式为Hf(0.15‑0.3)Zr(0.15‑0.3)Ce(0.15‑0.3)Y(0.05‑0.3)Al(0.05‑0.3)O2‑δ,该氧化物的制备方法包括以下步骤:(1)制备前驱体溶胶;(2)将前驱体溶胶烘干、研磨,得到前驱体凝胶粉;(3)将前驱体凝胶粉在900℃~1600℃保温1h~124h,制备出高温隔热高熵氧化物Hf(0.15‑0.3)Zr(0.15‑0.3)Ce(0.15‑0.3)Y(0.05‑0.3)Al(0.05‑0.3)O2‑δ粉体;该高熵氧化物具有稳定的Al‑O键,材料的高温稳定性好,采用溶胶凝胶法制备出的粉体均匀性较高,比表面积较高,制备的Hf(0.15‑0.3)Zr(0.15‑0.3)Ce(0.15‑0.3)Y(0.05‑0.3)Al(0.05‑0.3)O2‑δ粉体高温稳定性好,能够作为优异的高温隔热涂层。
Description
技术领域
本发明涉及一种高熵氧化物及其制备方法,更具体地,涉及一种高温隔热高熵氧化物及其制备方法。
背景技术
热障涂层广泛应用于重型燃气轮机及航空发动机等的热端部件,现有热障涂层材料多为氧化钇稳定氧化锆(掺杂YSZ)、稀土掺杂锆酸盐和磷酸盐等。随着重型燃气轮机和航空发动机的不断发展,其热端部件面临日益苛刻的服役环境,对热障涂层材料的热导率、高温热稳定性和热机械性能等提出了更高要求。高熵陶瓷材料具有更低的热导率,因此引起了众多的关注,文献From high-entropy ceramics to compositionally-complexceramics:A case study of fluorite oxides和High-entropy fluorite oxides记载了利用氧化物获得一系列萤石型结构的高熵陶瓷粉末。然而,现有萤石型高熵陶瓷氧化物广泛采用稀有元素,材料的长期高温稳定性未见报导。
发明内容
发明目的:本发明的目的是提供一种含铝高温热稳定性好、相稳定性好、隔热性能好的高温隔热高熵氧化物,本发明的另一目的是提供该高熵氧化物的制备方法。
技术方案:本发明所述的高温隔热高熵氧化物,氧化物化学式为Hf(0.15-0.3)Zr(0.15-0.3)Ce(0.15-0.3)Y(0.05-0.3)Al(0.05-0.3)O2-δ,晶体结构为单一立方萤石相,组成元素均匀分布。
本发明所述的高温隔热高熵氧化物的制备方法,包括以下步骤:
(1)制备前驱体:先将酒精与四氯化铪、八水氧氯化锆、六水硝酸铈、六水硝酸钇和铝源混合并搅拌均匀,加入有机酸抑制金属盐水解,再加入适量较大粘度的有机物防止聚沉,搅拌加热至澄清,形成溶胶前驱体溶胶;
(2)将前驱体溶胶烘干、研磨,得到前驱体凝胶粉;
(3)将前驱体凝胶粉在900℃~1600℃保温1h~124h,制备出高温隔热高熵氧化物Hf(0.15-0.3)Zr(0.15-0.3)Ce(0.15-0.3)Y(0.05-0.3)Al(0.05-0.3)O2-δ粉体。
其中,步骤(1)中四氯化铪、八水氧氯化锆、六水硝酸铈、六水硝酸钇和铝源摩尔比为0.15~0.3:0.15~0.3:0.15~0.3:0.05~0.3:0.05~0.3;铝源为为六水氯化铝、无水氯化铝、九水硝酸铝或乙酰丙酮铝;酒精、金属盐总质量、有机酸和聚乙二醇的质量比为2~16:1:0.5~5:0.2~3;有机酸为柠檬酸、氨基磺酸、羟基乙酸或乙二胺四乙酸;有机物为聚乙二醇、甲基纤维素、聚乙烯吡络烷酮、树脂。
合成原理:采用无水乙醇为溶剂,同时加入了少量含水或不含水的有机酸如柠檬酸,使整个溶液呈现酸性,有效抑制了金属盐中Ce4+、Zr4+、Hf4+、Y3+、Al3+离子的水解,使金属阳离子能够在溶液中稳定存在;再加入有机物如聚乙二醇提高溶液粘度,使金属离子与柠檬酸络合后均匀分布、不易发生聚沉;通过不断加热搅拌浓缩,形成了稳定、均一、透明的溶胶;将溶胶缓慢烘干形成凝胶粉末,在此过程中,原料金属盐中阴离子((NO3)-,Cl-)裂解或挥发排出,溶液粘度逐渐增大,金属阳离子均匀分布,不存在偏析,仍均匀分布;凝胶粉活性高,通过控制凝胶粉末的热处理温度及时间、可有效控制颗粒尺寸。
有益效果:本发明与现有技术相比,其显著优点是:1、高熵氧化物内具有稳定的Al-O键,更有利于含铝金属表面;2、采用溶胶凝胶法制备出的粉体均匀性较高,比表面积较高,元素均匀分布;3、制备操作简单、分散性好;4、粉末的高温稳定性好,可用于高温长时间应用;5、应用于含铝金属表面更具有优势。
附图说明
图1是实施例1中的高熵氧化物的XRD图;
图2是实施例2中的高熵氧化物的扫描电镜图;
图3是实施例3中的高熵氧化物的扫描电镜图;
图4是实施例3中的高熵氧化物的EDS mapping图;
图5是实施例4中的高熵氧化物的扫描电镜图。
具体实施方式
实施例1
(1)将60g酒精和金属盐:0.96g四氯化铪、0.97g八水氧氯化锆、1.30g六水硝酸铈、1.15g六水硝酸钇和0.72g六水氯化铝搅拌混合均匀,,再加入10g一水柠檬酸和5g聚乙二醇,在70℃搅拌均匀至澄清,得到溶胶前驱体;
(2)将溶胶前驱体放入烘箱中180℃干燥12h并研磨;
(3)将研磨后的溶胶前驱体置于马弗炉中,在1500℃下保温1h,得到(Hf0.2Zr0.2Ce0.2Y0.2Al0.2)O2-δ粉体,其XRD结果如图1所示,可以看出氧化物为单一萤石型结构,空间群为Fm-3m。
实施例2
(1)将60g酒精和金属盐:0.96g四氯化铪、0.97g八水氧氯化锆、1.30g六水硝酸铈、1.15g六水硝酸钇和0.72g六水氯化铝搅拌混合均匀,再加入15g一水柠檬酸和5g聚乙二醇,在70℃搅拌均匀至澄清,得到溶胶前驱体;
(2)将溶胶前驱体放入烘箱中150℃干燥24h并研磨;
(3)将研磨后的溶胶前驱体置于马弗炉中,在900℃下保温1h,得到(Hf0.2Zr0.2Ce0.2Y0.2Al0.2)O2-δ粉体,其形貌如图2所示,可以看出粉末颗粒尺寸在20-40nm之间,分散性较好。
实施例3
(1)将60g酒精和金属盐:0.96g四氯化铪、0.97g八水氧氯化锆、1.30g六水硝酸铈、1.15g六水硝酸钇和0.72g六水氯化铝搅拌混合均匀,再加入15g一水柠檬酸和5g聚乙二醇,在70℃搅拌均匀至澄清,得到溶胶前驱体;
(2)将溶胶前驱体放入烘箱中150℃干燥24h并研磨;
(3)将研磨后的溶胶前驱体置于马弗炉中,在1500℃下保温4h,得到(Hf0.2Zr0.2Ce0.2Y0.2Al0.2)O2-δ粉体,其形貌如图3,可以看出粉末颗粒尺寸在1-4μm之间,分散性较好,元素面分布如图4所示,可以看出元素均匀分布。
实施例4
(1)将60g酒精和金属盐:0.96g四氯化铪、0.97g八水氧氯化锆、1.30g六水硝酸铈、1.15g六水硝酸钇和0.72g六水氯化铝搅拌混合均匀,再加入15g一水柠檬酸和5g聚乙二醇,在70℃搅拌均匀至澄清,得到溶胶前驱体;
(2)将溶胶前驱体放入烘箱中150℃干燥24h并研磨;
(3)将研磨后的溶胶前驱体置于马弗炉中,在1500℃下保温124h,得到(Hf0.2Zr0.2Ce0.2Y0.2Al0.2)O2-δ粉体,其形貌如图5所示,可以看出,粉末颗粒在经过124h的热处理后,颗粒尺寸仍在在1-4μm之间,颗粒长大不明显,具有优秀的抗烧结性。
实施例5
(1)将80g酒精和金属盐:0.64g四氯化铪、0.64g八水氧氯化锆、0.87g六水硝酸铈、1.15g六水硝酸钇和0.24g六水氯化铝搅拌混合均匀,,再加入20g一水柠檬酸和10g聚乙二醇,在80℃搅拌均匀至澄清,得到溶胶前驱体;
(2)将溶胶前驱体放入烘箱中240℃干燥12h并研磨;
(3)将研磨后的溶胶前驱体置于马弗炉中,在1500℃下保温4h,得到(Hf0.2Zr0.2Ce0.2Y0.3Al0.1)O2-δ粉体。
实施例6
(1)将80g酒精金属盐:0.80g四氯化铪、0.81g八水氧氯化锆、1.09g六水硝酸铈、0.48g六水硝酸钇和0.30g六水氯化铝搅拌混合均匀,再加入20g一水柠檬酸和10g聚乙二醇,在80℃搅拌均匀至澄清,得到溶胶前驱体;
(2)将溶胶前驱体放入烘箱中90℃干燥24h并研磨;
(3)将研磨后的溶胶前驱体置于马弗炉中,在1500℃下保温4h,得到(Hf0.25Zr0.25Ce0.25Y0.125Al0.125)O2-δ粉体。
实施例7
(1)将80g酒精金属盐:0.80g四氯化铪、0.81g八水氧氯化锆、1.09g六水硝酸铈、0.67g六水硝酸钇和0.18g六水氯化铝搅拌混合均匀,再加入20g一水柠檬酸和10g聚乙二醇,在80℃搅拌均匀至澄清,得到溶胶前驱体;
(2)将溶胶前驱体放入烘箱中90℃干燥24h并研磨;
(3)将研磨后的溶胶前驱体置于马弗炉中,在1500℃下保温4h,得到(Hf0.25Zr0.25Ce0.25Y0.175Al0.075)O2-δ粉体。
实施例8
(1)将80g酒精金属盐:0.91g四氯化铪、0.92g八水氧氯化锆、1.23g六水硝酸铈、0.28g六水硝酸钇和0.18g六水氯化铝搅拌混合均匀,再加入20g一水柠檬酸和10g聚乙二醇,在80℃搅拌均匀至澄清,得到溶胶前驱体;
(2)将溶胶前驱体放入烘箱中90℃干燥24h并研磨;
(3)将研磨后的溶胶前驱体置于马弗炉中,在1500℃下保温4h,得到(Hf0.284Zr0.28 4Ce0.284Y0.074Al0.074)O2-δ粉体。
实施例9
(1)将80g酒精金属盐:0.81g四氯化铪、0.92g八水氧氯化锆、1.23g六水硝酸铈、0.38g六水硝酸钇和0.12g六水氯化铝搅拌混合均匀,再加入20g一水柠檬酸和10g聚乙二醇,在80℃搅拌均匀至澄清,得到溶胶前驱体;
(2)将溶胶前驱体放入烘箱中90℃干燥24h并研磨;
(3)将研磨后的溶胶前驱体置于马弗炉中,在1500℃下保温4h,得到(Hf0.284Zr0.28 4Ce0.284Y0.01Al0.005)O2-δ粉体。
上述实施例的基础上还可以进行其他形式的变化或者变动,这里不对所有的实施例进行列举,凡是属于本发明的技术方案所以发的技术方案的显而易见的变化仍在本发明的保护范围。
对比例1
(1)将80g酒精金属盐:0.64g四氯化铪、0.64g八水氧氯化锆、0.87g六水硝酸铈、0.19g六水硝酸钇和0.84g六水氯化铝搅拌混合均匀,再加入20g一水柠檬酸和10g聚乙二醇,在80℃搅拌均匀至澄清,得到溶胶前驱体;
(2)将溶胶前驱体放入烘箱中90℃干燥24h并研磨;
(3)将研磨后的溶胶前驱体置于马弗炉中,在1500℃下保温4h。
热处理后,晶相不再是单相缺陷萤石型,不能得到(Hf0.2Zr0.2Ce0.2Y0.05Al0.35)O2-δ粉体。
Claims (7)
1.一种高温隔热高熵氧化物,其特征在于,所述氧化物化学式为Hf(0.15-0.3)Zr(0.15-0.3)Ce(0.15-0.3)Y(0.05-0.3)Al(0.05-0.3)O2-δ,晶体结构为单一立方萤石相,组成元素均匀分布。
2.一种权利要求1所述的高温隔热高熵氧化物的制备方法,其特征在于,包括以下步骤:
(1)制备前驱体:先将酒精与四氯化铪、八水氧氯化锆、六水硝酸铈、六水硝酸钇和铝源混合并搅拌均匀,加入有机酸抑制金属盐水解,再加入适量较大粘度的有机物防止聚沉,搅拌加热至澄清,形成前驱体溶胶;
(2)将前驱体溶胶烘干、研磨,得到前驱体凝胶粉;
(3)将前驱体凝胶粉在900℃~1600℃保温1h~124h,制备出高温隔热高熵氧化物Hf(0.15-0.3)Zr(0.15-0.3)Ce(0.15-0.3)Y(0.05-0.3)Al(0.05-0.3)O2-δ粉体。
3.根据权利要求2所述的高温隔热高熵氧化物的制备方法,其特征在于,所述步骤(1)中四氯化铪、八水氧氯化锆、六水硝酸铈、六水硝酸钇和铝源摩尔比为0.15~0.3:0.15~0.3:0.15~0.3:0.05~0.3:0.05~0.3。
4.根据权利要求2或3所述的高温隔热高熵氧化物的制备方法,其特征在于,所述步骤(1)中铝源为六水氯化铝、无水氯化铝、九水硝酸铝或乙酰丙酮铝。
5.根据权利要求2所述的高温隔热高熵氧化物的制备方法,其特征在于,步骤(1)中酒精、金属盐总质量、有机酸和有机物聚乙二醇的质量比为2~16:1:0.5~5:0.2~3。
6.根据权利要求2所述的高温隔热高熵氧化物的制备方法,其特征在于,所述步骤(1)中有机酸为柠檬酸、氨基磺酸、羟基乙酸或乙二胺四乙酸。
7.根据权利要求2所述的高温隔热高熵氧化物的制备方法,其特征在于,所述步骤(1)中有机物为聚乙二醇、甲基纤维素、聚乙烯吡络烷酮、树脂。
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