CN116161975A - 一种高断裂韧性的六方磁铅石结构高熵热障涂层材料及其制备方法 - Google Patents

一种高断裂韧性的六方磁铅石结构高熵热障涂层材料及其制备方法 Download PDF

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CN116161975A
CN116161975A CN202310296366.7A CN202310296366A CN116161975A CN 116161975 A CN116161975 A CN 116161975A CN 202310296366 A CN202310296366 A CN 202310296366A CN 116161975 A CN116161975 A CN 116161975A
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靳洪允
李开云
罗学维
黄烁
侯书恩
洪建和
袁硕果
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China University of Geosciences
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Abstract

本发明的一种高断裂韧性的六方磁铅石结构高熵热障涂层材料及其制备方法。化学组成式为LnMAl11O19，Ln位是(La0.2Nd0.2Sm0.2Eu0.2Gd0.2)，M位为Zn或Mg。制备方法：S1，按照化学组成式称取金属元素氧化物后混合湿法球磨；S2，将球磨后的物料过滤清洗后干燥；S3，将干燥后的粉末预烧后再煅烧。本发明根据原子尺寸差和质量差计算，在满足形成单相固溶体的条件下，筛选出Ln位是(La0.2Nd0.2Sm0.2Eu0.2Gd0.2)的LnMAl11O19，显著提高六方磁铅石结构的断裂韧性，且掺杂后生成的物相在高温下也十分稳定，不会产生杂相，对六方磁铅石结构的综合性能提升明显。

Description

一种高断裂韧性的六方磁铅石结构高熵热障涂层材料及其制 备方法
技术领域
本发明涉及热障涂层材料技术领域，尤其涉及一种高断裂韧性的六方磁铅石结构高熵热障涂层材料及其制备方法。
背景技术
热障涂层，又称隔热涂层，是一种陶瓷保护层，通过喷涂工艺将陶瓷沉积在热端部件表面，将部件与高温燃气隔离，利用陶瓷的低导热性，使高温燃气和工件金属基体之间产生很大的温降，使其免受高温氧化、腐蚀或者磨损，以达到保护热端部件、提高燃气热效率和延长使用寿命的目的。然而在热障涂层材料系统中，陶瓷涂层与基体材料在热循环过程中裂纹扩展使热障涂层材料剥落。因此，陶瓷涂层与基体材料的界面黏附、热/残余应力等对使热障涂层材料的使用寿命和可靠性至关重要。在高温热循环过程中，热力不匹配造成热障涂层产生裂纹。传统的热障涂层材料的断裂韧性较低，抵抗裂纹失稳扩展能力较差，致使涂层剥落失效，从而降低涂层的热循环寿命，已经越来越难以满足实际应用的需求。
发明内容
本发明的目的在于，针对现有技术的上述不足，提出一种高断裂韧性的六方磁铅石结构高熵热障涂层材料及其制备方法。
本发明的一种高断裂韧性的六方磁铅石结构高熵热障涂层材料，其化学组成式为LnMAl11O19，Ln位是(La0.2Nd0.2Sm0.2Eu0.2Gd0.2)，M位为Zn或Mg。
一种如上述的高断裂韧性的六方磁铅石结构高熵热障涂层材料的制备方法，包括以下步骤：
S1，按照化学组成式称取物料La2O3、Nd2O3、Sm2O3、Eu2O3、Gd2O3、纳米ZnO、Al2O3或MgO后混合湿法球磨；
S2，将球磨后的物料过滤清洗后干燥；
S3，将干燥后的粉末在一定温度下预烧一段时间，然后再一定温度下煅烧一段时间，即得高断裂韧性的六方磁铅石结构高熵热障涂层材料。
进一步的，步骤S3中，预烧温度为850～1000℃，时间为6～10h。。
进一步的，步骤S3中，煅烧温度为1400～1600℃，煅烧时间为至少5h。
进一步的，步骤S1中，将称取的物料放入球磨罐中，加入球磨珠，最后加入酒精，将球磨罐放入球磨机中，一定转速球磨5～7次，每次球磨用时1.5～2.5h，共计时长11～13h。
进一步的，球磨珠中，大珠：小珠＝1:1.5。
进一步的，过滤采用200目的筛网对物料进行过滤；清洗采用酒精反复冲洗筛网上的研磨珠直至冲洗后的酒精呈透明色为止。
进一步的，干燥温度为70～90℃，干燥时间96h以上。
本发明根据原子尺寸差和质量差计算，在满足形成单相固溶体的条件下，筛选出Ln位是(La0.2Nd0.2Sm0.2Eu0.2Gd0.2)的LnMAl11O19，提供了一种新的掺杂体系并显著提高六方磁铅石结构的断裂韧性，且掺杂后生成的物相在高温下也十分稳定，不会产生杂相，对六方磁铅石结构的综合性能提升明显。
本发明使用已经成熟使用的球磨法制备粉体，成本相对较低，通过对工艺参数的调控，获得的粉体具有较好的断裂韧性。
附图说明
图1为本发明中实施例1中(La0.2Nd0.2Sm0.2Eu0.2Gd0.2)ZnAl11O19粉体在1500℃下煅烧10h后XRD物相分析；
图2为本发明实施例2中(La0.2Nd0.2Sm0.2Eu0.2Gd0.2)ZnAl11O19粉体在1600℃保温10h后的显微组织；
图3为本发明实施例2中(La0.2Nd0.2Sm0.2Eu0.2Gd0.2)ZnAl11O19和实施例4中(La0.2Nd0.2Sm0.2Eu0.2Gd0.2)MgAl11O19的力学性能；
图4为本发明中实施例3中(La0.2Nd0.2Sm0.2Eu0.2Gd0.2)MgAl11O19粉体在1500℃下煅烧10h后XRD物相分析；
图5为本发明实施例4中(La0.2Nd0.2Sm0.2Eu0.2Gd0.2)MgAl11O19粉体在1600℃保温10h后的显微组织；
图6为本发明中实施例5中(La0.2Nd0.2Sm0.2Eu0.2Gd0.2)MgAl11O19粉体在1600℃下煅烧30h后XRD物相分析。
具体实施方式
以下是本发明的具体实施例并结合附图，对本发明的技术方案作进一步的描述，但本发明并不限于这些实施例。
实施例1
根据组成式为LnMAl11O19所表示的化合物，Ln位是(La0.2Nd0.2Sm0.2Eu0.2Gd0.2)，M位是Zn，将La2O3、Nd2O3、Sm2O3、Eu2O3、Gd2O3、纳米ZnO和Al2O3分别称量好放入球磨罐中，加入球磨珠(大珠：小珠＝1:1.5)，最后加入酒精；将此球磨罐放入球磨机中，转速使用机器默认转速，循环次数为6次，每次循环用时2h，共计时长12h左右；球磨结束后，在蒸发皿上放上一个200目的筛网，对液体进行过滤，用酒精反复冲洗筛网上的研磨珠直至冲洗后的酒精呈透明色为止，将盛有液体的蒸发皿放入80℃干燥箱中，干燥96h以上；将干燥后的粉末在950℃预烧8h，然后在1500℃下煅烧10h，得到(La0.2Nd0.2Sm0.2Eu0.2Gd0.2)ZnAl11O19粉体。
图1为实施例1中(La0.2Nd0.2Sm0.2Eu0.2Gd0.2)ZnAl11O19粉体在1500℃下煅烧10h后XRD物相分析，可以看出掺杂后的粉末物相稳定，没有产生杂相。
实施例2
根据组成式为LnMAl11O19所表示的化合物，Ln位是(La0.2Nd0.2Sm0.2Eu0.2Gd0.2)，M位是Zn，将La2O3、Nd2O3、Sm2O3、Eu2O3、Gd2O3、纳米ZnO和Al2O3分别称量好放入球磨罐中，加入球磨珠(大珠：小珠＝1:1.5)，最后加入酒精；将此球磨罐放入球磨机中，转速使用机器默认转速，循环次数为6次，每次循环用时2h，共计时长12h左右；球磨结束后，在蒸发皿上放上一个200目的筛网，对液体进行过滤，用酒精反复冲洗筛网上的研磨珠直至冲洗后的酒精呈透明色为止，将盛有液体的蒸发皿放入80℃干燥箱中，干燥96h以上；将干燥后的粉末在850℃预烧10h，然后在1600℃下煅烧10h，得到(La0.2Nd0.2Sm0.2Eu0.2Gd0.2)ZnAl11O19粉体。将得到的粉体以100℃/min的升温速率，在20MPa,1550℃的条件下保温5min进行放电等离子烧结，然后将表面磨抛，进行断裂韧性测试。
图2为实施例2中(La0.2Nd0.2Sm0.2Eu0.2Gd0.2)ZnAl11O19在1600℃保温10h后的显微组织，表面组织相互缠绕镶嵌在一起，其力学性能较好，由图3可以看出，(La0.2Nd0.2Sm0.2Eu0.2Gd0.2)ZnAl11O19硬度较高，断裂韧性也较大，其压痕硬度和弹性模量均略高于(La0.2Nd0.2Sm0.2Eu0.2Gd0.2)MgAl11O19，然而(La0.2Nd0.2Sm0.2Eu0.2Gd0.2)ZnAl11O19的断裂韧性为2.48MPa·m1/2，比(La0.2Nd0.2Sm0.2Eu0.2Gd0.2)MgAl11O19高出27％。并且(La0.2Nd0.2Sm0.2Eu0.2Gd0.2)ZnAl11O19的断裂韧性与8YSZ相当，比LZ及其高熵锆酸盐均优秀。
实施例3
根据组成式为LnMAl11O19所表示的化合物，Ln位是(La0.2Nd0.2Sm0.2Eu0.2Gd0.2)，M位是Mg，将La2O3、Nd2O3、Sm2O3、Eu2O3、Gd2O3、纳米MgO和Al2O3分别称量好放入球磨罐中，加入球磨珠(大珠：小珠＝1:1.5)，最后加入酒精；将此球磨罐放入球磨机中，转速使用机器默认转速，循环次数为6次，每次循环用时2h，共计时长12h左右；球磨结束后，在蒸发皿上放上一个200目的筛网，对液体进行过滤，用酒精反复冲洗筛网上的研磨珠直至冲洗后的酒精呈透明色为止，将盛有液体的蒸发皿放入80℃干燥箱中，干燥96h以上；将干燥后的粉末在950℃预烧8h，然后在1500℃下煅烧10h，得到(La0.2Nd0.2Sm0.2Eu0.2Gd0.2)MgAl11O19粉体。
图4为实施例3中(La0.2Nd0.2Sm0.2Eu0.2Gd0.2)MgAl11O19粉体在1500℃下煅烧10h后XRD物相分析，可以看出掺杂后的粉末物相稳定，没有产生杂相。
实施例4
根据组成式为LnMAl11O19所表示的化合物，Ln位是(La0.2Nd0.2Sm0.2Eu0.2Gd0.2)，M位是Mg，将La2O3、Nd2O3、Sm2O3、Eu2O3、Gd2O3、纳米MgO和Al2O3分别称量好放入球磨罐中，加入球磨珠(大珠：小珠＝1:1.5)，最后加入酒精；将此球磨罐放入球磨机中，转速使用机器默认转速，循环次数为6次，每次循环用时2h，共计时长12h左右；球磨结束后，在蒸发皿上放上一个200目的筛网，对液体进行过滤，用酒精反复冲洗筛网上的研磨珠直至冲洗后的酒精呈透明色为止，将盛有液体的蒸发皿放入80℃干燥箱中，干燥96h以上；将干燥后的粉末在850℃预烧10h，然后在1600℃下煅烧10h，得到(La0.2Nd0.2Sm0.2Eu0.2Gd0.2)MgAl11O19粉体。将得到的粉体以100℃/min的升温速率，在20MPa,1550℃的条件下保温5min进行放电等离子烧结，然后将表面磨抛，进行断裂韧性测试。
图5为实施例4中(La0.2Nd0.2Sm0.2Eu0.2Gd0.2)MgAl11O19在1600℃保温10h后的显微组织，表面组织相互缠绕镶嵌在一起，可以看出(La0.2Nd0.2Sm0.2Eu0.2Gd0.2)MgAl11O19力学性能较好，由图3可以看出，(La0.2Nd0.2Sm0.2Eu0.2Gd0.2)MgAl11O19硬度较高，断裂韧性较大。
实施例5
根据组成式为LnMAl11O19所表示的化合物，Ln位是(La0.2Nd0.2Sm0.2Eu0.2Gd0.2)，M位是Mg，将La2O3、Nd2O3、Sm2O3、Eu2O3、Gd2O3、纳米MgO和Al2O3分别称量好放入球磨罐中，加入球磨珠(大珠：小珠＝1:1.5)，最后加入酒精；将此球磨罐放入球磨机中，转速使用机器默认转速，循环次数为6次，每次循环用时2h，共计时长12h左右；球磨结束后，在蒸发皿上放上一个200目的筛网，对液体进行过滤，用酒精反复冲洗筛网上的研磨珠直至冲洗后的酒精呈透明色为止，将盛有液体的蒸发皿放入80℃干燥箱中，干燥96h以上；将干燥后的粉末在1000℃预烧6h，然后在1600℃下煅烧30h，得到(La0.2Nd0.2Sm0.2Eu0.2Gd0.2)MgAl11O19粉体。
图6为实施例5中(La0.2Nd0.2Sm0.2Eu0.2Gd0.2)MgAl11O19粉体在1600℃下煅烧30h后XRD物相分析，可以看出掺杂后的粉末物相稳定，没有产生杂相。
实施例6
根据组成式为LnMAl11O19所表示的化合物，Ln位是(La0.2Nd0.2Sm0.2Eu0.2Gd0.2)，M位是Zn，将La2O3、Nd2O3、Sm2O3、Eu2O3、Gd2O3、纳米ZnO和Al2O3分别称量好放入球磨罐中，加入球磨珠(大珠：小珠＝1:1.5)，最后加入酒精；将此球磨罐放入球磨机中，转速使用机器默认转速，循环次数为6次，每次循环用时2h，共计时长12h左右；球磨结束后，在蒸发皿上放上一个200目的筛网，对液体进行过滤，用酒精反复冲洗筛网上的研磨珠直至冲洗后的酒精呈透明色为止，将盛有液体的蒸发皿放入80℃干燥箱中，干燥96h以上；将干燥后的粉末在1000℃预烧10h，然后在1400℃下煅烧5h，得到(La0.2Nd0.2Sm0.2Eu0.2Gd0.2)ZnAl11O19粉体。得到的粉体经XRD物相分析，粉末物相稳定，没有产生杂相。
以上未涉及之处，适用于现有技术。
虽然已经通过示例对本发明的一些特定实施例进行了详细说明，但是本领域的技术人员应该理解，以上示例仅是为了进行说明，而不是为了限制本发明的范围，本发明所属技术领域的技术人员可以对所描述的具体实施例来做出各种各样的修改或补充或采用类似的方式替代，但并不会偏离本发明的方向或者超越所附权利要求书所定义的范围。本领域的技术人员应该理解，凡是依据本发明的技术实质对以上实施方式所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围。

Claims (8)

1.一种高断裂韧性的六方磁铅石结构高熵热障涂层材料，其特征在于，其化学组成式为LnMAl11O19，Ln位是(La0.2Nd0.2Sm0.2Eu0.2Gd0.2)，M位为Zn或Mg。
2.一种如权利要求1所述的高断裂韧性的六方磁铅石结构高熵热障涂层材料的制备方法，其特征在于，包括以下步骤：
S1，按照化学组成式称取物料La2O3、Nd2O3、Sm2O3、Eu2O3、Gd2O3、纳米ZnO、Al2O3或MgO后混合湿法球磨；
S2，将球磨后的物料过滤清洗后干燥；
S3，将干燥后的粉末在一定温度下预烧一段时间，然后再一定温度下煅烧一段时间，即得高断裂韧性的六方磁铅石结构高熵热障涂层材料。
3.如权利要求2所述的制备方法，其特征在于，步骤S3中，预烧温度为850～1000℃，时间为6～10h。
4.如权利要求2所述的制备方法，其特征在于，步骤S3中，煅烧温度为1400～1600℃，煅烧时间为至少5h。
5.如权利要求2所述的制备方法，其特征在于，步骤S1中，将称取的物料放入球磨罐中，加入球磨珠，最后加入酒精，将球磨罐放入球磨机中，一定转速球磨5～7次，每次球磨用时1.5～2.5h，共计时长11～13h。
6.如权利要求2所述的制备方法，其特征在于，球磨珠中，大珠：小珠＝1:1.5。
7.如权利要求2所述的制备方法，其特征在于，过滤采用200目的筛网对物料进行过滤；清洗采用酒精反复冲洗筛网上的研磨珠直至冲洗后的酒精呈透明色为止。
8.如权利要求2所述的制备方法，其特征在于，干燥温度为70～90℃，干燥时间96h以上。
CN202310296366.7A 2023-03-22 2023-03-22 一种高断裂韧性的六方磁铅石结构高熵热障涂层材料及其制备方法 Pending CN116161975A (zh)

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