硅酸盐学报

热循环处理对（Gd_0.9Yb_0.1）₂Zr₂O₇/Yb₂O₃稳定ZrO₂热障涂层力学性能的影响

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何永香 ¹^,² , 范习之 ¹^,² , 迟光芳 ¹^,² , 张伟 ¹^,² , 左劲旅 ³ , 李沙 ³ , 杨波 ³ , 毛卫国 ¹^,²

硅酸盐学报 | 研究论文 2024,52(7): 2329-2340

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硅酸盐学报 |研究论文 2024 , 52 (7) : 2329 -2340

热循环处理对（Gd_0.9Yb_0.1）₂Zr₂O₇/Yb₂O₃稳定ZrO₂热障涂层力学性能的影响

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何永香¹^,², 范习之¹^,², 迟光芳¹^,², 张伟¹^,², 左劲旅³, 李沙³, 杨波³, 毛卫国¹^,²

作者信息

^1．长沙理工大学材料科学与工程学院，长沙 410114

^2．高端装备先进涂层技术湖南省重点实验室，长沙 410114

^3．湖南博云新材料股份有限公司，长沙 410205

通讯作者:

毛卫国（1979—），男，博士，教授。

作者简介:

何永香（1998—），女，硕士研究生。

Effect of Heat-Treatment on Mechanical Properties of (Gd_0.9Yb_0.1)₂Zr₂O₇/Yb₂O₃ Stabilized ZrO₂ Coatings During Thermal Cycling

Yongxiang HE¹^,², Xizhi FAN¹^,², Guangfang CHI¹^,², Wei ZHANG¹^,², Jinlv ZUO³, Sha LI³, Bo YANG³, Weiguo MAO¹^,²

Affiliations

^1.College of Materials Science and Engineering, Changsha University of Science and Technology, Changsha 410114, China

^2.Hunan Provincial Key Laboratory of Advanced Coating Technology for High-End Equipment, Changsha 410114, China

^3.Hunan Boyun New Materials Corporation Limited, Changsha 410205, China

Corresponding Author:

MAO Weiguo (1979-), male, Ph.D., Professor. E-mail: ssamao@126.com

HE Yongxiang (1998-), female, Master candidate. E-mail: 1981775721@qq.com

出版时间: 2024-07-20 doi: 10.14062/j.issn.0454-5648.20240040

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摘要

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新型掺杂改性的锆酸钆涂层材料有望成为下一代航空发动机热端部件的关键防热材料。采用大气等离子喷涂工艺，在Inconel 600基底上制备了（Gd_0.9Yb_0.1）₂Zr₂O₇/Y₂O₃稳定ZrO₂（GYbZ/8YSZ）热障涂层，在1 100 ℃完成了100次热循环处理，系统分析了涂层成分、微观结构和力学性能的演变。结果表明，在喷涂前后和后期的热循环处理过程中，GYbZ材料结构稳定；在涂层界面产生了热生长氧化层，其逐渐增厚至20 μm；在50次热循环后，涂层弹性模量与硬度分别达到最大值182.01 GPa和9.13 GPa；高温原位压痕测试表明，在700 ℃后，GYbZ涂层表面高温硬度基本趋于稳定。经过不同次数热循环处理后，涂层残余应力变化范围为-41.02~ -123.67 MPa，断裂韧性范围为0.93~2.02 MPa·m^1/2。系统地讨论了高温长时间热处理过程中GYbZ/8YSZ体系微观结构演变与力学性能的关联，为后续可靠性预测提供了重要的实验依据。

关键词

热障涂层 / 氧化镱掺杂锆酸钆 / 高温硬度 / 断裂韧性 / 残余应力

Abstract

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Introduction

Thermal barrier coatings can be used for the stable operation of aircraft engines under high-temperature environments due to their excellent oxidation resistance, corrosion resistance and heat insulation properties. However, the high-temperature phase transition of conventional 8.0% (in mass fraction) Y₂O₃ stabilized ZrO₂ ceramic (8YSZ) materials exists when the service temperature exceeds 1 200 ℃. Developing thermal barrier coatings, such as rare-earth zirconates and rare-earth silicate, becomes popular. (Gd_0.9Yb_0.1)₂Zr₂O₇ (GYbZ)/8YSZ coatings with a low thermal conductivity and a high temperature phase stabilization are regarded as potential thermal protective materials. At present, some work focus on the preparation properties optimization of air plasma spraying, electron beam physical vapor deposition and plasma spray physical vapor deposition techniques, respectively. It is important to in-situ investigate the mechanical properties and failure mechanisms of GYbZ/8YSZ coatings at > 1 200 ℃.

Methods

GYbZ/8YSZ thermal barrier coatings were prepared with NiCrAlY, 8YSZ and GYbZ powders on an Inconel 600 nickel-based superalloy with the thickness of 2 mm via air plasma spraying. GYbZ/8YSZ thermal barrier coatings were subjected to thermal cycle treatments in a Muffle furnace at 1 100 ℃ for 1 h, and then cooled to room temperature for 1 thermal cycle. The times of thermal cycles were 10, 50 and 100, respectively. The phase and microstructure of the coatings were analyzed by X-ray diffraction (XRD) and scanning electron microscopy (SEM) before and after heat-treatments. The elastic modulus, hardness, fracture toughness and residual stress were measured by an indentation method at different temperatures.

Results and discussion

The XRD patterns show that GYbZ powder and the as-sprayed coating are a defective fluorite structure, and the doping of Yb³⁺ with small ionic radius makes the material change from a pyrochrite structure to a defective fluorite structure. In addition, the samples treated for different thermal cycles all maintain a defective fluorite structure, indicating that GYbZ has an excellent high-temperature phase stability. The SEM images show that the surface of the as-sprayed GYbZ coating has a good melting state, and massive micro-cracks are distributed on the surface, which is caused due to the quenching stress generated by the molten spray particles during the preparation process and the thermal stress generated by the mismatch between the thermal expansion coefficients between the layers. The bonding between the layers of GYbZ/8YSZ coatings is good, and the bonding interface is clear without any cracks. There are tiny pores in the interior. The distribution of elements in each layer is consistent with the design. After thermal cycling, the crack width of the coating surface gradually widens and the porosity gradually decreases. The thermal growth oxide (TGO) produced between the bond layer and the 8YSZ layer gradually increases, and the TGO grows to 20 μm after 100 thermal cycles. The generation of TGO leads to a large amount of stress concentration, leading to the initiation and rapid expansion of transverse cracks in the bonding layer and 8YSZ, and damages the structural stability of the GYbZ/8YSZ coatings. Also, some vertical cracks occur in GYbZ layer and 8YSZ layer. The results of element distribution test show that the oxygen content in the bond layer increases gradually with the increase of the number of thermal cycles. The creation of vertical cracks in the coating promotes the diffusion of oxygen, thus accelerating the growth of heat-grown oxides.

The results of mechanical properties test show that the elastic modulus and hardness of GYbZ/8YSZ coatings surface firstly increase and then decrease with the increase of thermal cycle, and have the maximum values at 50 thermal cycles. After thermal cycling, the coating is sintered and its densification is improved, resulting in an increase in the elastic modulus and hardness. After 100 thermal cycles, the coating oxidation is serious, the binding force between coatings is weakened, massive vertical cracks occur in the coating, the coating structure is damaged, the deformation resistance is weakened, and the elastic modulus and hardness are reduced. The hardness of the coating decreases from 5.09 GPa to 2.20 GPa from room temperature to 700 ℃. At 700-1 100 ℃, the hardness of the coating is 2.00 GPa. The residual stress of the as-sprayed coating is -41.02 MPa. The residual stress accumulates due to thermal expansion mismatch of coating system during thermal cycling. After 10 thermal cycles, the residual stress accumulates to-147.30 MPa. After 50 thermal cycles, the stress relaxation caused by cracks gradually reduces the residual stress. After 100 thermal cycles, the residual stress decreases to -105.92 MPa. The results show that the residual stress of the coating before and after thermal cycling is a compressive stress. The fracture toughness of the as-sprayed GYbZ coating is 0.93 MPa·m^1/2. The fracture toughness of the coating firstly increases and then decreases with the increase of the number of thermal cycles, and has a maximum value of 2.02 MPa·m^1/2 after 50 thermal cycles. After heat-treatment, the pores of the coating reduce, and the dense area and the compressive stress can prevent the crack propagation. Some microcracks can increase the strain tolerance of the coating to a certain extent, and enhance the fracture toughness of the coating. After 100 thermal cycles, oxidation and massive destructive cracks lead to the instability of the coating structure, the increase of defects and the decline of performance.

Conclusions

The pore distribution in the as-sprayed GYbZ/8YSZ coatings was uniform, and the bonding interface of each layer was clear. Before and after thermal cycling, GYbZ coating was a defective fluorite structure and had an excellent high-temperature stability. The density of the coating increased with the increase of the number of thermal cycle, occurring some transverse and vertical cracks, and the TGO thickness grew to 20 μm. After 50 thermal cycles, the elastic modulus and hardness reached the maximum values, which were 182.01 GPa and 9.13 GPa, respectively. From room temperature to 700 ℃, the coating hardness reduced to 2.20 GPa. At 700-1 100 ℃, the coating hardness was 2.00 GPa. During the thermal cycle, the residual stress of the coating varied from -41.02 MPa to -123.67 MPa, and the fracture toughness varied from 0.93 MPa·m^1/2 to 2.02 MPa·m^1/2.

Key words

thermal barrier coatings / ytterbium oxide doped gadolinium zirconate / high-temperature hardness / fracture toughness / residual stress

引用本文

何永香, 范习之, 迟光芳, 张伟, 左劲旅, 李沙, 杨波, 毛卫国. 热循环处理对（Gd_0.9Yb_0.1）₂Zr₂O₇/Yb₂O₃稳定ZrO₂热障涂层力学性能的影响. 硅酸盐学报, 2024 , 52 (7) : 2329 -2340 . DOI: 10.14062/j.issn.0454-5648.20240040

Yongxiang HE, Xizhi FAN, Guangfang CHI, Wei ZHANG, Jinlv ZUO, Sha LI, Bo YANG, Weiguo MAO. Effect of Heat-Treatment on Mechanical Properties of (Gd_0.9Yb_0.1)₂Zr₂O₇/Yb₂O₃ Stabilized ZrO₂ Coatings During Thermal Cycling[J]. Journal of the Chinese Ceramic Society, 2024 , 52 (7) : 2329 -2340 . DOI: 10.14062/j.issn.0454-5648.20240040

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国家重点研发计划(2021YFB3702304-4)
国家科技重大专项(J2019-VI-0017-0132; J2022-VI-0008-0039)
博云新材航天用先进碳基耐烧蚀材料领域创新团队

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2024年第52卷第7期

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文章信息

doi: 10.14062/j.issn.0454-5648.20240040

接收时间：2024-01-16
首发时间：2026-10-22
出版时间：2024-07-20

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收稿日期：2024-01-16
修回日期：2024-02-25

基金

国家重点研发计划(2021YFB3702304-4)

国家科技重大专项(J2019-VI-0017-0132; J2022-VI-0008-0039)

博云新材航天用先进碳基耐烧蚀材料领域创新团队

作者信息

^1．长沙理工大学材料科学与工程学院，长沙 410114

^2．高端装备先进涂层技术湖南省重点实验室，长沙 410114

^3．湖南博云新材料股份有限公司，长沙 410205

通讯作者:

毛卫国（1979—），男，博士，教授。

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https://castjournals.cast.org.cn/joweb/gsyxb/CN/10.14062/j.issn.0454-5648.20240040

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2种不同金属材料的力学参数

科 Family	属数 Number of genus	种数 Number of species	占总种数比例 Percentage of total species (%)	属 Genus	种数 Number of species	占总种数比例 Percentage of total species (%)
鹅膏菌科Amanitaceae	2	11	5.26	鹅膏菌属 Amanita	10	4.78
小菇科 Mycenaceae	2	12	5.74	丝盖伞属 Inocybe	5	2.39
多孔菌科 Polyporaceae	8	14	6.70	蜡蘑属 Laccaria	5	2.39
红菇科 Russulaceae	3	23	11.00	小皮伞属 Marasmius	6	2.87
				小菇属 Mycena	11	5.26
				光柄菇属 Pluteus	5	2.39
				红菇属 Russula	17	8.13
				栓菌属 Trametes	5	2.39

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